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At least 1,243 records · Page 69

Status on Microstructural Studies of Nuclear Graphite

This report documents the completion of the Advanced Reactor Technologies (ART) Level 3 Milestone (M3AT-26OR0605054), “Provide status on microstructural studies of nuclear graphite,” due May 1, 2026. The contents of this report summarize recent progress in the development of the Nuclear Graphite Microstructure Library, including datasets that have been generated, curated, and submitted for publication, as part of the broader effort to establish and integrate the library within the NDMAS platform.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Supplementary material for manuscript: Microcomputed X-ray Tomographic Imaging and Image Processing for Microstructural Characterization of Explosives

This data contains the supplemental information that will be accessible to the public from the paper “Microcomputed X-ray Tomographic Imaging and Image Processing for Microstructural Characterization of Explosives”. The data set contains the reconstructed slices for the 3D images of three different high explosives including: HMX-HTPB, PBX 9501 and PBX 9502. The data sets are folders of reconstructed tiffs showing the microstructure (crystals, binder, voids) and a segmented data set of each. Finally, a .gif movie is also present that plays the slices sequentially. The folders contain the voxel size information. See the manuscript for more details.

36 MATERIALS SCIENCE↗

Microstructure, electrical resistivity, and tensile properties of neutron-irradiated Cu–Cr–Nb–Zr

High strength, high conductivity copper alloys that can resist creep at high temperatures are one of the primary candidates for efficient heat exchangers in fusion reactors. Cu–Cr–Nb–Zr (CCNZ) alloys, which were designed to improve the strength and creep life of ITER Cu–Cr–Zr (CCZ) reference alloys, have been found to have comparable electrical conductivity and tensile properties to CCZ alloys. The measured creep rupture times for these improved alloys is about ten times higher than the ITER reference alloys at 90–125 MPa at 500 °C. However, the effects of neutron irradiation on these alloys, and the ensuing material properties, have not been studied; thus, their utility in a fusion reactor environment is not well understood. This study characterizes the room temperature mechanical and electrical properties of a neutron-irradiated CCNZ alloy and compares them to a neutron-irradiated ITER reference heat sink CCZ alloy. Tensile specimens were neutron irradiated in the High Flux Isotope Reactor (HFIR) to 5 dpa between 250 °C and 325 °C. Post-irradiation characterization included electrical resistivity measurements, hardness, and tensile tests. Microstructural evaluation used scanning electron microscopy, energy dispersive x-ray spectroscopy, and atom probe tomography to characterize the irradiation-produced changes in the microstructure and investigate the mechanistic processes leading to post-irradiation properties. Transmutation calculations were validated with composition measurements from atom probe data and used to calculate contributions to the increased electrical resistivity measured after irradiation. Comparisons with CCZ alloys in the same irradiation heat found that the post-irradiated CCNZ and CCZ alloys had comparable electrical resistivity. Although CCNZ alloys suffered more irradiation hardening than CCZ, the overall tensile behavior deviated very little from non-irradiated values in the temperature range studied.

36 MATERIALS SCIENCE↗

Large Area Detection of Microstructural Defects with Multi-Mode Ultrasonic Signals

Cyclic loading or other stresses can lead to development of cracks and crack growth in mechanical structures, leading to eventual failure. While ultrasound imaging can be used for non-destructive testing of such structures, conventional ultrasound techniques are often limited by crack size, density, and areal coverage. An effective characterization of real-world, large-area structures is required at an early damage stage to prevent catastrophic failure and predict remaining life. In this study, a new nonlinear ultrasonic testing (NUT) method is proposed for large-area monitoring of practical structures with arbitrary complexity by using multiple-mode guided-wave ultrasonic signals. The proposed guided-wave NUT technique requires single-element transducers, simple electronics, and a mixed time-frequency domain signal processing. As a proof-of-concept demonstration, numerical simulations and experiments are performed on an A36 carbon steel beam assembly with previously formed microstructural defects that cause nonlinearities in ultrasonic response. The quadratic dependence of the nonlinear wave excitation on the input ultrasonic signal amplitude is shown by numerical simulations, and such a nonlinear ultrasonic response is experimentally observed in the zone with a high density of microstructural defects.

36 MATERIALS SCIENCE↗

The Convolutional Multiple Whole Profile (CMWP) Fitting Method, a Global Optimization Procedure for Microstructure Determination

The analysis of line broadening in X-ray and neutron diffraction patterns using profile functions constructed on the basis of well-established physical principles and TEM observations of lattice defects has proven to be a powerful tool for characterizing microstructures in crystalline materials. These principles are applied in the convolutional multiple-whole-profile (CMWP) procedure to determine dislocation densities, crystallite size, stacking fault and twin boundary densities, and intergranular strains. The different lattice defect contributions to line broadening are separated by considering the hkl dependence of strain anisotropy, planar defect broadening and peak shifts, and the defect dependent profile shapes. The Levenberg–Marquardt (LM) peak fitting procedure can be used successfully to determine crystal defect types and densities as long as the diffraction patterns are relatively simple. However, in more complicated cases like hexagonal materials or multiple-phase patterns, using the LM procedure alone may cause uncertainties. Here, we extended the CMWP procedure by including a Monte Carlo statistical method where the LM and a Monte Carlo algorithm were combined in an alternating manner. The updated CMWP procedure eliminated uncertainties and provided global optimized parameters of the microstructure in good correlation with electron microscopy methods.

36 MATERIALS SCIENCE↗

Microstructural and Hall–Petch Analysis of Additively Manufactured Ferritic Alloy Using 2507 Duplex Stainless Steel Powder

The powder bed fusion–laser beam (PBF-LB) process, a method of additive manufacturing (AM), was used to print duplex stainless steel (DSS) using commercial-grade 2507 powders. While conventionally processed DSS has a two-phase microstructure consisting of 50% austenite and 50% ferrite, the PBF-LB-printed 2507 alloy was nearly 100% ferrite. Optimal processing conditions that minimized porosity were determined to be 290 W laser power and 1000 mm/s scan speed, and grain size, texture, and phases were characterized as a function of laser power and scan speed. Grain size increased with increasing laser power but decreased with increasing scan speed. A <100> texture diminished with increasing scan speed from 1000 mm/s to 1400 mm/s. No austenite phase was detected. Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) characterization revealed nanoscale chromium nitride precipitates in the ferritic matrix (incoherent hexagonal close-packed (HCP) precipitates at grain boundaries and coherent body-centered cubic (BCC) precipitates within the grains) and a high density of tangled dislocations. Tensile tests of as-printed alloys showed a yield strength of 570 MPa, an ultimate tensile strength of 756 MPa, and an elongation to failure of 10%. The tensile properties were analyzed based on the observed microstructure considering grain size, nanoscale precipitates, and the high density of dislocations.

Crystallography↗

Investigation of Three-Dimensional Microstructure of Tricalcium Silicate (C 3 S) by Electron Microscopy

A serial block-face scanning electron microscopy (SBFSEM) system, composed of a scanning electron microscope (SEM) and an ultra-microtome installed within the SEM vacuum chamber, has been used to characterize the three-dimensional (3D) microstructure of tricalcium silicate (C 3 S) grains embedded in epoxy resin. A selection of C 3 S grains were segmented and rendered with 3D-image processing software, which allowed the C 3 S grains to be clearly visualized and enabled statistically quantitative analysis. The results show that about 5% of the C 3 S grains have volumes larger than 1 μm 3 and the average volume of the grains is 25 μm 3 . Pores can also be clearly seen in the biggest C 3 S grain, the volume of which is 3.6 × 10 4 μm 3 , and the mean volume and total volume of all the pores within this grain are 4.8 μm 3 and 3.0 × 10 3 μm 3 , respectively. This work provides a new approach for the characterization of the 3D spatial structure of raw C 3 S materials, and the resulting 3D structure of the raw C 3 S is important for further systematic research on the relationships between the spatial microstructure and the hydration kinetics of C 3 S and other cement minerals.

36 MATERIALS SCIENCE↗

An Overview of Nano Multilayers as Model Systems for Developing Nanoscale Microstructures

The microstructural transformations of binary nanometallic multilayers (NMMs) to equiaxed nanostructured materials were explored by characterizing a variety of nanoscale multilayer films. Four material systems of multilayer films, Hf-Ti, Ta-Hf, W-Cr, and Mo-Au, were synthesized by magnetron sputtering, heat treated at 1000 °C, and subsequently characterized by transmission electron microscopy. Binary systems were selected based on thermodynamic models predicting stable nanograin formation with similar global compositions around 20–30 at.%. All NMMs maintained nanocrystalline grain sizes after evolution into an equiaxed structure, where the systems with highly mobile incoherent interfaces or higher energy interfaces showed a more significant increase in grain size. Furthermore, varying segregation behaviors were observed, including grain boundary (GB) segregation, precipitation, and intermetallic formation depending on the material system selected. The pathway to tailored microstructures was found to be governed by key mechanisms and factors as determined by a film’s initial characteristics, including global and local composition, interface energy, layer structure, and material selection. This work presents a global evaluation of NMM systems and demonstrates their utility as foundation materials to promote tailored nanomaterials.

Appleget, Chelsea D.↗

Cost-Effective Thermomechanical Processing of Nanostructured Ferritic Alloys: Microstructure and Mechanical Properties Investigation

Nanostructured ferritic alloys (NFAs), such as oxide-dispersion strengthened (ODS) alloys, play a vital role in advanced fission and fusion reactors, offering superior properties when incorporating nanoparticles under irradiation. Despite their importance, the high cost of mass-producing NFAs through mechanical milling presents a challenge. This study delves into the microstructure-mechanical property correlations of three NFAs produced using a novel, cost-effective approach combining severe plastic deformation (SPD) with the continuous thermomechanical processing (CTMP) method. Analysis using scanning electron microscopy (SEM)-electron backscatter diffraction (EBSD) revealed nano-grain structures and phases, while scanning transmission electron microscopy (STEM)-energy dispersive X-ray spectroscopy (EDS) quantified the size and density of Ti-N, Y-O, and Cr-O fine particles. Atom probe tomography (APT) further confirmed the absence of finer Y-O particles and characterized the chemical composition of the particles, suggesting possible nitride dispersion strengthening. Correlation of microstructure and mechanical testing results revealed that CTMP alloys, despite having lower nanoparticle densities, exhibit strength and ductility comparable to mechanically milled ODS alloys, likely due to their fine grain structure. However, higher nanoparticle densities may be necessary to prevent cavity swelling under high-temperature irradiation and helium gas production. Further enhancements in uniform nanoparticle distribution and increased sink strength are recommended to mitigate cavity swelling, advancing their suitability for nuclear applications.

36 MATERIALS SCIENCE↗

Microstructure and Magnetic Properties of Grain Refined Pr2Co14B Melt-Spun Ribbons

The correlation between the grain refining effect of TiC on the microstructure of Pr2Co14B melt-spun ribbons and the magnetic properties is presented in this study. TiC enabled greater control of microstructure both in the as-spun and heat treated Pr2Co14B, compared with the material without TiC. As a result, coercivity of the sample with TiC was nearly twice that of the sample without TiC. In addition to Pr2Co14B, two other phases were found in the sample with TiC: one rich in Co and the other having a composition near PrCo2. TiC was found near the grain boundaries and at triple junctions. Also no Ti or C was found in the matrix phase indicating extreme low solubility of the elements when both are present with Pr2Co14B. As expected, both the samples with and without TiC have similar anisotropy field but the presence of room temperature non-ferromagnetic phases (TiC and PrCo2), caused a small decrease in magnetization of the sample with TiC although the romance of the isotropic materials were comparable.

36 MATERIALS SCIENCE↗

Enhancement of γ/γ’ Microstructured Cobalt Superalloys Produced from Atomized Powder by Creating a Harmonic Structure

A material’s properties must be continuously improved to meet the demands of extreme conditions in high-temperature applications. It is demonstrated that γ-γ’ Co-based superalloys could surpass the yield stress of Ni-based superalloys at high temperature due to the γ-γ’ structure. The powders were subjected to a harmonic modification in order to refine the grain structure on the surface and to activate the sintering process. This study examines how harmonic structure affects microstructure and mechanical properties at high temperatures. Spark Plasma Sintering (SPS) was used for consolidation to maintain the ultrafine grain size microstructure of the powder. Compression tests were conducted from room temperature (RT) to 750 °C to assess the mechanical properties of the material. Yield stress values obtained from harmonic structures are four times higher than those obtained from cast alloys.

36 MATERIALS SCIENCE↗

Advanced Geomechanical Model to Predict the Impact of CO2-Induced Microstructural Alterations on the Cohesive-Frictional Behavior of Mt. Simon Sandstone

We investigated the influence of CO2-induced geochemical reactions on the cohesive-frictional properties of host rock within the context of CO2 storage in a saline aquifer and focused on the Mt. Simon sandstone. The research objective was to model geo-mechanical changes due to host rock exposure to CO2-saturated brine while accounting for heterogeneity, double-scale porosity, and granular structure. We formulated a three-level multi-scale model for host rocks. We conducted scanning electron microscopy analyses to probe the microstructure and grid nanoindentation to measure the mechanical response. We derived new nonlinear strength upscaling solutions to correlate the effective strength characteristics and the macroscopic yield surface to the micro-structure at the nano-, micro-, and meso-scales. Specifically, our theoretical model links CO2-induced microstructural alterations to a reduction in the size of the yield surface, and a drop in the value of the friction coefficient. In turn, regarding the Illinois Basin Decatur Project, the CO2-induced drop in friction coefficient is linked to an increase in the risk of fault slip and a higher probability of induced microseismicity during and after the end of CO2 underground injection operations. The theoretical model presented is essential for the geo-mechanical modeling of CO2 underground injection operations at multiple length-scales.

58 GEOSCIENCES↗

Through-Thickness Microstructure Characterization in a Centrifugally Cast Austenitic Stainless Steel Nuclear Reactor Primary Loop Pipe Using Time-of-Flight Neutron Diffraction

The US code of Federal Regulations mandates regular inspection of centrifugally cast austenitic stainless steel pipe, commonly used in primary cooling loops in light-water nuclear power plants. These pipes typically have a wall thickness of ~8 cm. Unfortunately, inspection using conventional ultrasonic techniques is not reliable as the microstructure strongly attenuates ultrasonic waves. Work is ongoing to simulate the behavior of acoustic waves in this microstructure and ultimately develop an acoustic inspection method for reactor inspections. In order to account for elastic anisotropy in the material, the texture in the steel was measured as a function of radial distance though the pipe wall. Experiments were conducted on two 10 × 12.7 × 80 mm radial sections of a cast pipe using neutron diffraction scans of 2 mm slices using the HIPPO time-of-flight neutron diffractometer at the Los Alamos Neutron Science Center (LANSCE, Los Alamos, NM, USA). Strong textures dominated by a small number of austenite grains with their (100) direction aligned in the radial direction of the pipe were observed. ODF analysis indicated that up to 70% of the probed volume was occupied by just three single-grain orientations, consistent with grain sizes of almost 1 cm. Texture and phase fraction of both ferrite and austenite phases were measured along the length of the samples. These results will inform the development of a more robust diagnostic tool for regular inspection of this material.

42 ENGINEERING↗

Multi‐scale simulation of rock compaction through breakage models with microstructure evolution

Abstract. Regional subsidence due to fluid depletion includes the interaction among multiple physical processes. Specifically, rock compaction is governed by coupled hydro-mechanical feedbacks involving fluid flow, effective stress change and pore collapse. Although poroelastic models are often used to explain the delay between depletion and subsidence, recent evidence indicates that inelastic effects could alter the rock microstructure, thus exacerbating coupling effects. Here, a constitutive law built within the framework of Breakage Mechanics is proposed to account for the inherent connection between rock microstructure, hydraulic conductivity, and pore compaction. Furthermore, it is embedded into a 1-D hydromechanical coupled finite element analysis (FEA) to explore the effects of micro-structure rearrangement on the development of reservoir compaction. Numerical examples with the proposed model are compared with simulations under constant hydraulic conductivity to illustrate the model capability to capture the non-linear processes of reservoir compaction induced by fluid depletion.

Buscarnera, Giuseppe↗

Cloud microstructure as determined by an optical cloud particle spectrometer.

Use of an improved single-particle light-scattering instrument for measurement of cloud microstructure in field studies. Cloud particle size and number information is measured over 12 sizing intervals, in the range from 4 to 85 microns in diameter. The microstructure can be observed in real time and with a spatial resolution not previously reported. The general features of water cloud droplet size and number distributions are consistent with previous direct capture and replication studies. The transition from water to ice phase regions in cumuliform clouds can be inferred from dramatic changes observed in the distribution features. Results are also presented for stratus and cirrus cloud penetrations.

Ryan, R. T.↗

A study of the microstructure and optical properties of thin lead-dielectric cermet films

A transmission electron microscopy study involving direct and replicating techniques is directed to a definition of the microstructure of radio frequency-sputtered, thin lead-dielectric cermet films. Once defined, this microstructure is used to obtain theoretical film refractive indices. The Maxwell Garnett theory provides a basis for the theoretical results. Measurements of film transmission and reflectivity are used to obtain rough experimental values for film refractive indices by the Tekucheva method. More exact values are obtained via ellipsometry. The rough Tekucheva values are used to determine the range over which computer calculations interpreting the ellipsometric results must be made. This technique yields accurate values for the film refractive indices.

Owen, R. B.↗

The effect of microstructure on the fracture toughness of titanium alloys

The microstructure of the alpha titanium alloy Ti-5Al-2.5Sn and the metastable beta titanium alloy Beta 3 was examined. The material was from normal and extra low interstitial grade plates which were either air-cooled or furnace-cooled from an annealing treatment. Beta 3 was studied in alpha-aged and omega-aged plates which were heat treated to similar strength levels. Tensile and plane strain fracture toughness tests were conducted at room temperature on the alpha-aged material. The microstructure and fracture mechanisms of alloys were studied using optical metallography, electron microscopy, microprobe analyses, and texture pole figures. Future experiments are described.

Vanstone, R. H.↗

Exponential kinetics of formation of organic microstructures

Organic microstructure production in Miller-Urey spark discharge flasks is an energy-dependent, autocatalytic process which follows first order kinetics similar to microbial growth curves. These relationships hold for all three major morphological types of microstructures observed. The three types are assembled from smaller precursor subunits which associate according to a binomial distribution. These structures could have formed bounded systems in which pre-biological processes might have occurred.

Fraser, C. L.↗