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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Microstructure-Based Understanding of High-Temperature Deformation Behaviors in Laser Powder Bed Fusion (LPBF) 316H Stainless Steel

This report presents the results of high-temperature mechanical property testing and microstructural analysis of laser powder bed fusion (LPBF) 316H stainless steel (SS) conducted during Fiscal Year 2025 (FY25) under the U.S. Department of Energy, Office of Nuclear Energy’s Advanced Materials and Manufacturing Technologies (AMMT) program. The study builds upon prior work by expanding the mechanical property test matrix and advancing a microstructure-based mechanistic understanding of LPBF 316H SS performance, with a focus on the solution annealed (SA, 1100°C for 1 hour) materials. High-temperature tension, creep, fatigue, and creep-fatigue tests were performed. Thermal aging studies were conducted. Advanced characterization techniques, including scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), and high-energy synchrotron X-ray diffraction, were employed to investigate the microstructural evolution during thermal aging and mechanical testing. It was discovered that the as-built (AB) LPBF 316H SS exhibited precipitation kinetics during thermal aging that are 10–100 times faster than its wrought counterpart due to the presence of high densities of preferred nucleation sites, while the precipitation kinetics in SA LPBF 316H was under investigation. The accelerated precipitation of embrittling phases such as sigma phase in LPBF 316H SS compared to its wrought counterpart led to significant impacts on creep ductility. The influence of laser printing parameters and build orientations on fatigue and creep-fatigue performance was observed. In assessing the creep-fatigue performance, it was discovered that the SA LPBF 316H samples failed in less than 200 cycles under 595°C, 0.5% (strain amplitude) with a 60-minute hold time. This work establishes a mechanistic framework for predicting the long-term behavior of LPBF 316H SS, supporting its rapid qualification under the ASME BPVC. The findings contribute to the broader goal of enabling the deployment of advanced materials in next-generation nuclear energy systems. An outlook for FY26 work, including continued aging studies, mechanical testing, and microstructural characterization, is provided.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Automated piezoresponse force microscopy domain tracking during fast thermally stimulated phase transition in CuInP 2 S 6

Real-time tracking of dynamic nanoscale processes such as phase transitions by scanning probe microscopy is a challenging task, typically requiring extensive and laborious human supervision. Smart strategies to track specific regions of interest (ROI) in the system during such transformations in a fast and automated manner are necessary to study the evolution of the microscopic changes in such dynamic systems. In this work, we realize automated ROI tracking in piezoresponse force microscopy during a fast (≈0.8 °C s –1 ) thermally stimulated ferroelectric-to-paraelectric phase transition in CuInP 2 S 6 . We use a combination of fast (1 frame per second) sparse scanning with compressed sensing image reconstruction and real-time offset correction via phase cross correlation. The applied methodology enables in situ fast and automated functional nanoscale characterization of a certain ROI during external stimulation that generates sample drift and changes local functionality.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Resolving atomic transport through iron oxide under irradiation using isotopic tracers

Structural materials in nuclear environments are exposed to complex and harsh conditions, including high temperatures, corrosive solutions, and irradiation. Material stability and likewise degradation are fundamentally controlled by atomic transport mechanisms. Here, we investigate the influence of radiation-induced, non-equilibrium point defect populations on mass transport within model oxide systems using isotopic tracers and atom probe tomography. An isotopically labelled hematite (a-Fe2O3) film was synthesized with 16O- and 18O-rich layers (>30nm and 10 nm, respectively) sequentially deposited via molecular beam epitaxy. One region of the film was proton irradiated to ~0.1 dpa at 450°C, and regions outside the beam spot provided a non-irradiated control of thermal annealing only. 3D APT was used to directly visualize the elemental and O-isotopic redistribution following both thermal and combined thermal and irradiation conditions. Complementary scanning transmission electron microscopy (STEM) was also employed to study the microstructural evolution. Error function fits of the 18O-concentration profiles enabled quantification of diffusion coefficients.

isotopic tracers, diffusion, proton irradiation, h↗
DOE OSTI2021

Epitaxial growth of monolayer PdTe 2 and patterned PtTe 2 by direct tellurization of Pd and Pt surfaces

Two-dimensional (2D) palladium ditelluride (PdTe 2 ) and platinum ditelluride (PtTe 2 ) are two Dirac semimetals, which have fascinating quantum properties such as superconductivity, magnetism and topological order and show the promising applications in future nanoelectronics and optoelectronics. However, the synthesis of PdTe 2 and PtTe 2 monolayers (MLs) is hindered by a strong interlayer coupling and orbital hybridization. Here, in this study, we demonstrate an efficient synthesis of PdTe 2 and PtTe 2 MLs Large-area and high quality MLs of PdTe 2 and patterned PtTe 2 were epitaxially grown on the Pd(111) and Pt(111) surfaces by direct telurization in ultra-high vacuum. This was confirmed by x-ray photoelectron spectroscopy, low energy electron diffraction and scanning tunnelling microscopy. PdTe 2 ML demonstrated high thermal stability showing no decomposition sign after annealing at 470 °C. A well-ordered (2 × 2) PtTe 2 structure with Kagome lattice was observed on Te/Pt(111) surface following annealing at 200 °C in UHV, where the (2 × 2) pattern was formed by Te atom vacancies. PtTe 2 multilayer film was prepared as well, and it demonstrated the excitation of the Dirac plasmons as measured by high-resolution electron energy loss spectroscopy. The direct tellurization offers the simple and reliable protocol for the preparation of the ML of PdTe 2 and patterned PtTe 2 , and this opens new opportunities for quantum phenomena research and for practical optoelectronics applications.

2D materials↗
DOE OSTI2023

Strong metal–support bonding enhanced thermal stability in Au–Al 2 O 3 core–shell nanowires characterized by in situ transmission electron microscopy

In this study, the thermal stability of Au–Al 2 O 3 core–shell and Au nanowires was investigated by in situ scanning transmission electron microscopy and other techniques. Here, the nanowires were synthesized by the helium droplets method and deposited on various substrates. The in situ characterization of Au–Al 2 O 3 thermal stability demonstrated a substantially enhanced stability as compared to that of pure Au nanowires, which can be a transformative approach to design more durable Au-based nanocatalysts. Our study also revealed the existence of strong metal–support bonding in the Au/Al 2 O 3 system.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Dynamics and structure of the B2→B19’ phase transformation in NiTi revealed through in situ 4D-STEM

The structural evolution of NiTi during the B2→B19’ martensitic phase transformation via thermal cycling is investigated using in situ four dimensional scanning transmission electron microscopy (4D-STEM). With 4D-STEM, we can directly visualize and quantify the nanoscale evolution of the martensitic structure on thermal cycling and also investigate the origin of diffuse scattering of NiTi in the pre-transitional state. Mapping of the martensite orientation and strain visualizes the progression of the transformation front and self-accommodation of the B19’ structure. Diffuse streaking and strain are measured in the pre-transitional austenite (B2) phase and demonstrate no localization or preferential directionality hinting that long-range homogeneous instability rather than nanoscale heterogeneities may be the origin of the pre-transitional anomalies in NiTi. Finally, it is revealed that NiTi does not reform the same martensite nanostructure on thermal cycling but does express similar features. This small variation is likely owing to transformation-induced dislocations.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Nanoscale mapping of point defect concentrations with $\mathrm{4D-STEM}$

Vacancies are missing atoms in a crystalline material, and occur both at equilibrium (varying with temperature) and out of equilibrium such as when crystalline materials are damaged with radiation or corrosion. While we know of their importance, particularly regarding diffusive mechanisms, it is not straightforward to experimentally measure their concentration or to visualize them directly. Traditionally, measurements such as positron annihilation spectroscopy and to some degree X-ray diffraction can measure average concentrations, but generally lack the ability to visualize or quantify a heterogenous concentration of vacancies that can occur at the level of individual defects and microstructural features. Here, we present a method to map vacancy concentrations and their distribution using local lattice parameter measurements with a high-resolution electron microscope. Our method utilizes a Au thin film as a model to demonstrate the method via four-dimensional scanning transmission electron microscopy (4D-STEM) by correlating the differences between changes in lattice parameter and the volumetric thermal expansion during in situ heating experiments. The vacancy mapping methodology is also applied to non-equilibrium defects accumulated in pure Al via knock-on electron beam irradiation. Our method demonstrates the ability to map point defect concentrations in heterogeneous systems in situ with nanometer spatial resolution. The result is a technique that can provide direct measurements of vacancy concentrations at the level of individual defects in studies of materials in and out of equilibrium.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Thermodynamic properties of Gd-Bi alloys determined by emf measurements in LiCl-KCl-GdCl 3 electrolyte

Thermodynamic properties of binary Gd-Bi alloys (mole fraction, x Gd = 0.02–0.35) were determined using electromotive force (emf) measurements in molten LiCl-KCl-GdCl 3 electrolyte in complement with structural, microstructural, and thermal characterization. X-ray diffractometry (XRD) and scanning electron microscopy (SEM) identified the phase constituents of Gd-Bi alloys (x Gd = 0.02–0.35) as Bi matrix and GdBi compound. According to differential scanning calorimetry (DSC) measurements up to 1250 K, a eutectic transition [L = Bi + GdBi] was observed at 543 K but the reported peritectic transition [L + GdBi = GdBi 2 ] was not detected, suggesting the absence of the GdBi 2 compound. Based on structural, microstructural, and thermal characterization of Gd-Bi alloys (x Gd = 0.02–0.35), the GdBi 2 compound was not detected, and its thermodynamic stability is questionable. The emf of Gd-Bi alloy (x Gd = 0.16) at 700–1048 K relative to Gd(s) was measured by electrodepositing pure Gd metal at 25 K increments. Further, the emf values of Gd-Bi alloys were determined via coulometric titration of Gd into liquid Bi using a two-phase [L + GdBi] alloy as a reference electrode at 773–973 K. The solubility of Gd in liquid Bi was also estimated to be 0.50 mol% (773 K), 0.99 mol% (873 K), and 2.21 mol% (973 K) and the excess partial molar Gibbs energy (Δ$\mathrm{\bar{G}^{ex}_{Gd}}$) of liquid Gd-Bi alloys was as low as 65 kJ mol –1 , indicating strong chemical interactions between Gd and Bi.

36 MATERIALS SCIENCE↗
DOE OSTI2022

An insight into microscopy and analytical techniques for morphological, structural, chemical, and thermal characterization of cellulose

Cellulose obtained from plants is a bio-polysaccharide and the most abundant organic polymer on earth that has immense household and industrial applications. Hence, the characterization of cellulose is important for determining its appropriate applications. In this article, we review the characterization of cellulose morphology, surface topography using microscopic techniques including optical microscopy, transmission electron microscopy, scanning electron microscopy, and atomic force microscopy. Additionally, other physicochemical characteristics like crystallinity, chemical composition, and thermal properties are studied using techniques including X-ray diffraction, Fourier transform infrared, Raman spectroscopy, nuclear magnetic resonance, differential scanning calorimetry, and thermogravimetric analysis. This review may contribute to the development of using cellulose as a low-cost raw material with anticipated physicochemical properties.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2024

Testing of Materials and Coatings at up to 1150°C and 300 bar for use in Oxy-Combustion Turbine

Various materials that may be used in a supercritical carbon dioxide (sCO2) oxy-fuel turbine in the 150-300 MWe size range are being evaluated in various environments of interest. The inlet of the turbine must be capable of 1,150 °C at 300 bar and the exhaust temperature is expected to be within the 725-775 °C range. The design requirements are pushing the known limits of high temperature materials. Little is known about the oxidation of the metallic alloys considered for turbine nozzles and blades or about the resilience of thermal management solutions, such as thermal barrier coatings (TBC), required to accommodate these high temperatures. The combinations of high temperature resistant materials and coatings must be tested in sCO2 to evaluate their reliability in an oxy-fuel turbine environment. A total of 13 alloys were chosen to be tested. They included bare samples, with nano deposited MCrAlY bond coat only, or with the addition of a TBC. A unique test facility was developed to expose those materials in sCO2 at up to 300 bar and 1150 °C for up to 5,000 hours. This was accomplished by placing an induction heater inside an autoclave to achieve those high temperature locally while the pressurized vessel is cooled externally. The specimens are weighed before and after exposure to determine the oxidation rate. The integrity, morphology, and composition of some of the coatings and thermally grown oxide will be investigated by scanning electron microscopy (SEM). This paper presents the up-to-date results of the testing coated and uncoated superalloys in sCO2 at up to 1150 °C and up to 300 bar performed at Southwest Research Institute.

Bocher, Florent↗
DOE OSTI2025

Quantifying the effects of artificial aging on the ignition and self-propagating reactions of Ni(V)/Al multilayers

Bimetallic, reactive multilayers are uniformly structured materials composed of alternating nanoscale layers that may be ignited to produce self-propagating intermetallic-formation reactions. When reactive multilayers age, there is a change in local composition and loss of stored chemical energy due to mass transport and rearrangement at the interfaces. Here, to quantify the long-term reliability of commercial Ni(V)/Al multilayers, the effects of accelerated aging on both ignition sensitivity and self-propagating reactions have been examined. Thermally aged samples were characterized using transmission electron microscopy, differential scanning calorimetry, and laser ignition combined with high-speed videography. The analytically quantifiable nature of both continuous wave laser ignition and reactive wave propagation enabled calculations of Arrhenius rate constants for as-received and various heat-treated multilayers. With heat treatment, there is a change in the intermixed thickness and interfacial chemistry that decreases the activation energy for point ignition but increases it for self-propagating reactions. This finding implies that with increased thermal aging, the reaction becomes easier to facilitate in the solid state but harder in the liquid phase.

Energetic material↗
DOE OSTI2024

Effects of Ionizing Radiation on the Thermodynamic Stability of Boehmite and Gibbsite

Here, in this study, we examined the effect of gamma radiation on the stabilities of aluminum hydroxide (gibbsite) and aluminum oxyhydroxide (boehmite) nanoparticles in relation to their thermal decomposition. X-ray diffraction (XRD) patterns and scanning electron microscopy (SEM) images revealed no significant differences in mineral components or morphology before and after radiation. However, thermogravimetric and differential scanning calorimetry (TGA/DSC) analyses showed that both boehmite and gibbsite nanoparticles experienced decreased mass loss following irradiation. Raman and attenuated total reflection-Fourier transfer infrared (ATR-FTIR) spectra indicated that a fraction of the hydroxyl content in both cases was selectively cleaved by radiation, primarily at the particle surfaces. Quantitative analyses of thermal mass loss behavior demonstrated that irradiated boehmite and gibbsite nanoparticles had higher activation energies than their pristine counterparts, with the extent of the increase dependent on the total dose. Taken together, these findings suggest that exposure to a sufficient dose of ionizing radiation alters these materials such that they are less prone to decomposition by dehydration. This increased stability may be due to the decreased hydrous nature of the samples after radiation exposure, which was supported by further high temperature drop calorimetry. Additionally, a radiation-induced amorphous phase on the nanoparticle surfaces appears to have a permanent and positive influence on their thermodynamic stabilities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Interrogating the Effects of Hydrogen on the Behavior of Planar Deformation Bands in Austenitic Stainless Steel

The effects of internal hydrogen on the deformation microstructures of 304L austenitic stainless steel have been characterized using electron backscattered diffraction (EBSD), transmission Kikuchi diffraction (TKD), high-resolution scanning transmission electron microscopy (HRSTEM), and nanoprobe diffraction. Samples, both thermally precharged with hydrogen and without thermal precharging, were subjected to tensile deformation of 5 and 20 pct true strain followed by multiple microscopic interrogations. Internal hydrogen produced widespread stacking faults within the as-forged initially unstrained material. While planar deformation bands developed with tensile strain in both the hydrogen-precharged and non-precharged material, the character of these bands changed with the presence of internal hydrogen. As shown by nanobeam diffraction and HRSTEM observations, in the absence of internal hydrogen, the bands were predominantly composed of twins, whereas for samples deformed in the presence of internal hydrogen, ε -martensite became more pronounced and the density of deformation bands increased. For the 20 pct strain condition, α '-martensite was observed at the intersection of ε -martensite bands in hydrogen-precharged samples, whereas in non-precharged samples α '-martensite was only observed along grain boundaries. We hypothesize that the increased prevalence of α '-martensite is a secondary effect of increased ε -martensite and deformation band density due to internal hydrogen and is not a signature of internal hydrogen itself.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Phase stability and microstructure of neutron-irradiated substoichiometric yttrium dihydrides

The impact of the neutron-displacement damage on phase stability and microstructure of substoichiometric yttrium dihydrides (YH x , x <2) were investigated to assess their use as solid moderator in high-temperature nuclear reactors. YH x specimens were, thus, subjected to neutron irradiations in the range of 0.1–2 displacements per yttrium atom (dpa-Y) in the temperature range of 536–878°C at the Oak Ridge National Laboratory's (ORNL's) High Flux Isotope Reactor (HFIR). YH x specimens were initially prepared at stoichiometry (H/Y) ratios of 1.69 and 1.83. HFIR-irradiated specimens were characterized by variety of techniques to investigate H retention characteristics including dimensional analysis, optical microscopy, scanning electron microscopy electron back scatter diffraction (EBSD), transmission electron microscopy, thermal desorption spectroscopy (TDS), and high-energy x-ray diffraction (HE-XRD) characterizations. Overall, YH x exhibited notable structural and phase stability under short-term neutron-irradiation, except for the samples with significant silicon carbide (SiC) interaction at high doses and temperatures. Basic dimensional and mass measurements were misleading for accurate assessment of H retention, as confirmed by EBSD phase maps, XRD line profiles, and TDS signals. Thus, it was discussed that a robust H retention metric is needed to assess irradiated hydrides. Further, nanoscale cavities were observed as a result of the neutron irradiation in all samples. Although no clear impact of dose and irradiation temperature was determined, the initial H/Y ratio had an impact on the cavity number density where low H/Y specimens had high-resistance to cavity formation. The Y-vacancy cluster formation at the collision stage of the displacement cascade and their stabilization by H were considered to be the likely underlying mechanisms for the observed cavity microstructure.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2024

Correlation of Processing and Structure in an Ethylene‐Glycol Side‐Chain Modified Polythiophene via Combined X‐Ray Scattering and 4D Scanning Transmission Electron Microscopy

The results of a combined grazing incidence wide-angle X-ray scattering (GIWAXS) and 4D scanning transmission microscopy (4D-STEM) analysis of the effects of thermal processing on poly(3[2-(2-methoxyethoxy)ethoxy]-methylthiophene-2,5-diyl) are reported, a conjugated semiconducting polymer used as the active layer in organic electrochemical transistor devices. GIWAXS provides a measure of overall crystallinity in the film, while 4D-STEM produces real-space maps of the morphology and orientation of individual crystallites along with their spatial extent and distribution. The sensitivity of the 4D-STEM detector allows for collection of electron diffraction patterns at each position in an image scan while limiting the imparted electron dose to below the damage threshold. In conclusion, the effects of heat treatment on the distribution and type of crystallites present in the films is determined.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Styrene-Based Elastomer Composites with Functionalized Graphene Oxide and Silica Nanofiber Fillers: Mechanical and Thermal Conductivity Properties

The mechanical and thermal conductivity properties of two composite elastomers were studied. Styrene–butadiene rubber (SBR) filled with functionalized graphene oxide (GO) and silica nanofibers, and styrene–butadiene–styrene (SBS) block copolymers filled with graphene oxide. For the SBR composites, GO fillers with two different surface functionalities were synthesized (cysteamine and dodecylamine) and dispersed in the SBR using mechanical and liquid mixing techniques. The hydrophilic cysteamine-based GO fillers were dispersed in the SBR by mechanical mixing, whereas the hydrophobic dodecylamine-based GO fillers were dispersed in the SBR by liquid mixing. Silica nanofibers (SnFs) were fabricated by electrospinning a sol–gel precursor solution. The surface chemistry of the functionalized fillers was studied in detail. The properties of the composites and the synergistic improvements between the GO and SnFs are presented. For the SBS composites, GO fillers were dispersed in the SBS elastomer at several weight percent loadings using liquid mixing. Characterization of the filler material and the composite elastomers was performed using x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, scanning electron microscopy, thermogravimetric analysis, dynamic mechanical analysis, tensile testing, nanoindentation, thermal conductivity and abrasion testing.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Composition-Dependent Reconstructions of Titanium Oxide Clusters and Cu(111) Support via Cluster-Adatom Interactions

Mass-selected cluster deposition and scanning tunneling microscopy (STM) were used to investigate the surface structure and thermal stability of Ti 3 O y (y = 5, 6) clusters on a Cu(111) surface. STM imaging shows that the substoichiometric Ti 3 O 5 clusters aggregate into large dendritic assemblies at step edges, while the stoichiometric Ti 3 O 6 clusters are highly dispersed as single or small groupings of clusters. Cluster deposition also results in extensive reconstruction of the Cu(111) surface. The Ti 3 O 5 /Cu(111) surface exhibits one Cu-layer deep pits that are ringed by cluster assemblies that nucleate and grow at the perimeter step edges. By comparison, the Ti 3 O 6 /Cu(111) surface consists of irregular step edges and small one Cu-layer islands that are decorated with clusters. The restructuring of the Cu(111) surface is attributed to strong Cu-cluster interactions that release Cu adatoms from the step edges. This mechanism is supported by density functional theory (DFT) calculations, which predict that the Cu adatom attachment to the clusters is energetically favorable. Annealing the surfaces at elevated temperatures (400-700 K) results in higher densities of irregular steps, pits and isolated Cu islands as well as increased cluster aggregation. In conclusion, this work highlights adatom-cluster interactions as another manifestation of strong cluster-support interactions that can significantly alter the nature of the oxide-metal interface.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2024

Impacts of Curing-Induced Phase Segregation in Silicon Nanoparticle-Based Electrodes

We report the investigation of silicon nanoparticle composite anodes for Li-ion batteries, using a combination of two nm-scale atomic force microscopy-based techniques: scanning spreading resistance microscopy for electrical conduction mapping and contact resonance and force volume for elastic modulus mapping, along with scanning electron microscopy-based energy dispersion spectroscopy, nanoindentation, and electrochemical analysis. Thermally curing the composite anode—made of polyethylene oxide-treated Si nanoparticles, carbon black, and polyimide binder—reportedly improves the anode electrochemical performance significantly. This work demonstrates phase segregation resulting from thermal curing, where alternating bands of carbon and silicon active material are observed. This electrode morphology is retained after extensive cycling, where the electrical conduction of the carbon-rich bands remains relatively unchanged, but the mechanical modulus of the bands decreases distinctly. These electrical and mechanical factors may contribute to performance improvement, with carbon bands serving as a mechanical buffer for Si deformation and providing electrical conduction pathways. This work motivates future efforts to engineer similar morphologies for mitigating capacity loss in silicon electrodes.

25 ENERGY STORAGE↗