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At least 235 records · Page 13

Ultrasonic additive manufacturing of zirconium: Pilot results

Ultrasonic additive manufacturing (UAM) was successfully applied to the Zirconium material system to create a three-dimensional component prototype. The UAM process resulted in grain size refinement and significant localized deformation. Electron backscatter diffraction analysis revealed activated slip systems only applicable at high deformation temperatures, while texture analysis showed a decrease in measurable texture of the UAM build in comparison to the initial Zr-foil. Average tensile strengths in the X (sonotrode travel), Y (vibration), and Z (build) directions averaged 435 MPa, 458 MPa, and 359 MPa, respectively, demonstrating the viability of UAM for Zr-based materials. Furthermore, the delamination of some Z specimens along foil boundaries during loading suggests an interplay between interfacial Ti impurities introduced during welding and the spatial dependence of weld quality for this material system.

36 MATERIALS SCIENCE↗

Unlocking superplasticity in medium and high-entropy alloys

Superplasticity, the capacity of materials to sustain extraordinary tensile elongations at elevated temperatures, underpins a range of advanced metal-forming technologies. Conventionally, it is achieved in fine-grained alloys where deformation is dominated by grain-boundary sliding, accommodated by diffusion and dislocation activity. The advent of medium- and high-entropy alloys (M/HEAs), with their high chemical complexity and unconventional phase stability, offers new pathways to superplastic behavior beyond traditional alloy systems. Although investigated only recently, several M/HEAs already exhibit elongations that rival or exceed those of classical superplastic materials, particularly when ultrafine or metastable microstructures are engineered. Here, we review progress in understanding superplastic deformation in M/HEAs, emphasizing the interplay among composition, initial microstructure, thermomechanical processing, and microstructural evolution during high-temperature deformation. We discuss approaches to generating the fine-grained structures necessary for grain-boundary sliding, including severe plastic deformation and tailored heat treatments. We further highlight dynamic phenomena such as phase transformations, evolving grain-boundary chemistry, and deformation-induced grain refinement that can enhance plasticity in these systems. These mechanisms often shift the balance of deformation processes, enabling large elongations even outside classical criteria. Finally, we outline key challenges for application, including cost, scalability, recyclability, and microstructural stability.

klenam, Desmond [University of the Witwatersrand, ↗

The role of pre-existing heterogeneities in materials under shock and spall

There has been a challenge for many decades to understand how heterogeneities influence the behavior of materials under shock loading, eventually leading to spall formation and failure. Experimental, analytical, and computational techniques have matured to the point where systematic studies of materials with complex microstructures under shock loading and the associated failure mechanisms are feasible. This is enabled by more accurate diagnostics as well as characterization methods. As interest in complex materials grows, understanding and predicting the role of heterogeneities in determining the dynamic behavior becomes crucial. Early computational studies, hydrocodes, in particular, historically preclude any irregularities in the form of defects and impurities in the material microstructure for the sake of simplification and to retain the hydrodynamic conservation equations. Contemporary computational methods, notably molecular dynamics simulations, can overcome this limitation by incorporating inhomogeneities albeit at a much lower length and time scale. This review discusses literature that has focused on investigating the role of various imperfections in the shock and spall behavior, emphasizing mainly heterogeneities such as second-phase particles, inclusions, and voids under both shock compression and release. Pre-existing defects are found in most engineering materials, ranging from thermodynamically necessary vacancies, to interstitial and dislocation, to microstructural features such as inclusions, second phase particles, voids, grain boundaries, and triple junctions. This literature review explores the interaction of these heterogeneities under shock loading during compression and release. Systematic characterization of material heterogeneities before and after shock loading, along with direct measurements of Hugoniot elastic limit and spall strength, allows for more generalized theories to be formulated. Further, continuous improvement toward time-resolved, in situ experimental data strengthens the ability to elucidate upon results gathered from simulations and analytical models, thus improving the overall ability to understand and predict how materials behave under dynamic loading.

36 MATERIALS SCIENCE↗

Effect of grain-boundary θ-Al 2 Cu precipitates on tensile and compressive creep properties of cast Al–Cu–Mn–Zr alloys

Tensile and compressive creep tests were performed at 300 °C on high-temperature Al–Cu–Mn–Zr (ACMZ) alloys with 6 wt% Cu (6Cu) and 9 wt% Cu (9Cu) to evaluate the effect on creep properties of micron-size θ-Al 2 Cu intergranular precipitates. For compressive creep, the increased volume fraction of θ-precipitates at grain boundaries (from ~0.7% in 6Cu to ~ 6% in 9Cu) does not affect deformation rates across the investigated stress range of 15–110 MPa, consistent with creep being controlled by submicron θ'-Al 2 Cu precipitates within grains, whose size and fractions are the same in both alloys. In contrast, for tensile creep, 9Cu creeps faster than 6Cu at stresses above 20 MPa, and this difference increases with the stress level. Additionally, this discrepancy between tensile and compressive creep behavior is explained by cavitation during tensile creep, which is favored by higher volume fraction and larger size of intergranular θ precipitates in 9Cu. Conversely, larger precipitates impede cavity linkage resulting in improved creep ductility of 9Cu as compared to 6Cu at 300 °C.

36 MATERIALS SCIENCE↗

10° off-axis testing of CFRP using DIC: A study on strength, strain and modulus

For the determination of the shear properties such as strength, strain and modulus of unidirectionally reinforced composites, nearly a dozen measurement techniques exist, several of which have found their way into standards. One non-standardized method for sheet materials is the 10° off-axis tensile test of unidirectional coupons. The current work focuses on the experimental investigation of tensile testing of CFRP-UD coupon specimens using the 10° off-axis test and DIC strain mapping to measure the full-field deformation response. A sensitivity analysis on the measured stresses, strains and moduli is performed by varying the aspect ratio of the specimens and the location of strain measurement. Test related uncertainties such as the loading angle and specimen preparation details are investigated and quantified with the help of these full-field DIC measurements.

42 ENGINEERING↗

2019 accomplishments: degradation of mechanical properties in structural metals and welds for FTS reservoirs

This report documents work in 2019 at SRNL in support of the Aging and Lifetimes program. Specimens for fracture toughness testing were prepared in prior years by thermally pre-charging samples, provided by Sandia National Laboratories, of welded types 304L and 21-6-9 stainless steels. These samples were pre-charged in 2017. The fracture toughness of the first aged specimens was measured and compared to historical data. The measurements of the 304L and 21-6-9 weld and particularly HAZ represent some of the first fracture data relevant to modern GTS reservoirs. This work represents an on-going collaboration between SRNL and SNL to understand tritium embrittlement of structural metals in Gas Transfer System reservoirs which informs lifetime assessments. Continued testing was conducted on ongoing historical studies, including the effects of very long-term aging, and the relative performance of differently forged stockpile relevant 304L and 316L samples. New samples were pre-charged with tritium and placed in a freezer for an aging study to allow helium to build into the material. The precharged samples consist of smooth and notched tensile samples of 304L stainless steel, as well as tube tensile samples of different thermal treatments supplied by Sandia National Laboratories. Their charging marks the beginning of a new sequence of studies to explore fundamental deformation mechanisms underpinning tritium embrittlement. At predesignated times, samples will be removed from aging and tested to provide data which will help develop an understanding of material degradation with increasing aging time. Also documented is progress in employing various advanced characterization techniques including high resolution electron microscopy, thermally programed desorption, and small angle x-ray scattering, as well as facilities renovations and equipment procurements in support of sustained tritium impacts on materials program at SRNL.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Multiscale modeling of shear banding in metallic glasses (Final report)

Metallic glasses (MGs) possess remarkably high strength but suffer from minimal tensile ductility due to the formation of catastrophic shear bands. The goal of this research project is to develop an understanding of the microstructures and deformation mechanisms that control shear banding in MGs, which will enable the development of MGs with enhanced plasticity. Two scientific objectives have been pursued. (1) Understand the underlying mechanisms of shear banding phenomena in presence of nanoscale heterogeneities in MGs. (2) Understand the evolution of MG heterogenous structure upon thermomechanical stimuli for plasticity enhancement through controlling and distributing multiple shear bands.

36 MATERIALS SCIENCE↗

Temperature-Dependent Mechanical Anisotropy in Textured Zircaloy Cladding

This work evaluates deformation activity in textured zircaloy-4 cladding with the aim of elucidating the mechanisms that govern mechanical behavior across a temperature range anticipated in reactor service. In particular, the dependence of mechanical anisotropy on temperature and stress state (ratio of applied stresses) is examined via uniaxial and biaxial tensile experiments at room temperature and 400 °C. The mechanical behavior was interpreted based on micro-texture and dominant slip system activity. Thermal activation of basal systems is found as a key mechanism affecting mechanical behavior across the temperature range. The biaxial stress states produce resolved shear stresses contrasting to uniaxial stress states. As a result, mechanical testing and implications for reactor pellet-cladding mechanical interaction stress conditions are discussed.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Thermal Conductivity of Graphene Coated Copper Under Uniaxial Tensile Mechanical Strain

Graphene continues to demonstrate promise as a highly effective barrier coating, even at only one atom thick. The thermal properties of this coating are also promising to allow diffusion of heat across the surface, as the isolated graphene is an intrinsically good thermal conductor, yet this and its behavior under mechanical deformation has been less extensively studied. This report demonstrates that the in-plane thermal conductivity and interfacial thermal conductance of graphene coatings on copper are affected by mechanical strain. By inducing a strain in the copper substrate, the Raman-active 2D peak exhibits a change in position as well as a change in laser power dependence as the copper substrate is uniaxially elongated to a maximum of 0.5%. Non-linear trends in thermal conductivity are observed with tensile strain in samples with differing strain transfer rates from the substrate, indicating the close correlation between intrinsic thermal conduction and interfacial properties in atomically thin coatings transferred onto metals.

36 MATERIALS SCIENCE↗

A correlation-based approach for evaluating mechanical properties of nuclear fuel cladding tubes

The present work offers and evaluates a correlation-based approach to determine the tensile properties of nuclear fuel cladding tubes. A set of model materials with known properties (i.e., austenitic and ferritic steels, fcc- and hcp-alloys) were tested to build a correlation between conventional tensile tests and ring (hoop) and tube (axial) tests. It was shown that close-to-linear relationships exist for the basic mechanical properties (i.e., yield and ultimate stress, uniform and total elongation) between the uniaxial tensile test data and the ring and tube test data. Using the ring and tube specimen geometries, the feasibility of the approach was demonstrated via manufacturing and testing specimens from irradiated Zr and FeCrAl nuclear fuel cladding tubes. Limitations caused by specific deformation mechanisms (e.g., high ductility of 304L steel) were discussed in detail. The approach can be extended to other tubular products with different geometry and dimensions.

36 MATERIALS SCIENCE↗

The effect of aspect ratio on the mechanical behavior of Li metal in solid-state cells

The Li metal anode is necessary for solid-state batteries to dramatically exceed the energy density of state-of-the-art conventional Li-ion batteries. To enable the Li metal anode, the mechanical properties of Li metal under compression in a commercially relevant cell configuration must be determined. This work examines the compression creep behavior of Li metal coupled with a relevant model solid-state electrolyte (Li 6.5 La 3 Ta 0.5 Zr 1.5 O 12 ) and current collector (Ni) as a function of applied stress (1–10 MPa) and Li foil thickness (100–700 μm). At 1 MPa applied stress, the strain rate of all Li foil thicknesses under compression was almost four orders of magnitude lower than what is predicted from tensile creep tests. Steady-state creep behavior was observed for Li foil ≥350 μm at 5 MPa and ≥250 μm at 10 MPa. Conversely, sustained creep deformation was not observed for 100 and 150 μm Li foils at any applied stress. It is suggested that friction at the Li/LLZO and Li/Ni interfaces leads to the formation of hydrostatic stress that controls Li deformation at low aspect ratios. Finally, these results have implications for battery pack stack pressure requirements, particularly relating to void formation during stripping and Li metal filament penetration during plating.

25 ENERGY STORAGE↗

Microstructure and mechanical behavior of a TiC nanoprecipitate strengthened V Alloy

The V-4Cr-4Ti (V44) alloys have been proposed as the prime candidate structural material for self-cooled liquid Li blanket and other designs for fusion energy applications. However, the applications of the V44 alloy are limited to a narrow operation temperature window, due to reduction in creep strength at or above 700 °C and susceptibility to irradiation hardening and embrittlement when irradiated below 400 °C. Here, in this work, we explore the feasibility of designing a novel V alloy to form a high number density of TiC nanoprecipitates, in order to simultaneously improve creep strength and provide defect sinks to mitigate irradiation hardening. Computational thermodynamics was used to design a new alloy (V44C) to achieve our goal of high TiC nanoprecipitates density within the alloy V44 matrix. To ensure scalability, the new alloy was made through arc-melting and ingot-casting followed by hot forging, cold rolling and heat treatments of homogenization and precipitation aging. The microstructure was characterized by SEM, TEM, XRD and APT, confirming the existence of nanoprecipitates predicted in the thermodynamic calculations. In addition to microstructural evaluation tensile properties at room temperature and 700 °C, and Charpy impact energy at room temperature were measured. The microstructure and mechanical properties were then compared with those from a historic reference V44 alloy. The tensile strength improvement in V44C was rationalized based on particle and solid solution strengthening mechanism. The fracture behavior was discussed based on the fractography results and necking deformation behavior.

Alloys development↗

The {10$\overline{1}$2} non-cozone twin-twin interactions in Mg: A stability and mobility study using 3-D atomistic simulations

Due to easy activation of tensile twinning in Mg, multiple {10$\overline{1}$2} twin variants can interact with each other and form twin-twin boundaries over the course of plastic deformation. Previous studies using 2-D settings provide only a partial understanding of these interactions, especially the non-cozone ones. Here, atomistic simulations are used to study the 3-D structural characteristic and evolution of the non-cozone {10$\overline{1}$2} twin-twin junctions. The study reveals the existence of new twin-twin boundaries (TTBs) such as TTB BP and TTB K2 , formed after the interaction between the basal prismatic and conjugate twin interfaces with the coherent twin boundary. Here, for both non-cozone twin-twin interactions, the {10$\overline{1}$2} TTB and its associated twin-twin junctions are found to play a major role in the {10$\overline{1}$2} twin's stability and mobility. Specifically, they promote the growth of the 3-D twin in both the normal and forward directions during the interaction and hinder the detwinning process upon unloading.

36 MATERIALS SCIENCE↗

Fracture and fatigue of thin crystalline SrTiO 3 membranes

The increasing availability of a variety of two-dimensional materials has generated enormous growth in the field of nanoengineering and nanomechanics. Recent developments in thin film synthesis have enabled the fabrication of freestanding functional oxide membranes that can be readily incorporated in nanomechanical devices. While many oxides are extremely brittle in bulk, recent studies have shown that, in thin membrane form, they can be much more robust to fracture as compared to their bulk counterparts. Here, we investigate the ultimate tensile strength of SrTiO 3 membranes by probing freestanding SrTiO 3 drumheads using an atomic force microscope. We demonstrate that SrTiO 3 membranes can withstand an elastic deformation with an average strain of ~6% in the sub-20 nm thickness regime, which is more than an order of magnitude beyond the bulk limit. Further, we also show that these membranes are highly resilient upon a high cycle fatigue test, surviving up to a billion cycles of force modulation at 85% of their fracture strain, demonstrating their high potential for use in nanomechanical applications.

36 MATERIALS SCIENCE↗

Experimental Evaluation of Deformation and Fracture Mechanisms in Highly Irradiated Austenitic Steels

The present report documents recent experimental results of analysis using scanning electron microscopy/electron backscatter diffraction (SEM-EBSD) of plastic deformation mechanisms and strain localization phenomena in austenitic steels irradiated by neutrons. Experiments were performed with specimens irradiated to 125 dpa and, additionally, with specimens that experienced radiation-induced swelling up to 3%. Section 1 briefly analyzes the deformation localization in irradiated steels and its consequences on the material performance. The section describes the advantages and importance of the SEM-EBSD approach combined with in situ mechanical testing capability. Section 2 briefly introduces the experimental tools and methods (i.e., SEM/EBSD in situ tensile frame, electric discharge machine to manufacture irradiated specimens) and describes the investigated materials (i.e., element composition, irradiation conditions, and general microstructure). Section 3 describes the key experimental results and provides a brief analysis and comparison with the datasets obtained earlier within the same task (i.e., low-dose specimens). The discussion focuses on EBSD microstructure maps with strain localization features, misorientation evolution as a function of strain, and observed deformation mechanisms. Section 4 evaluates data collected in recent years on highly irradiated steel and estimates the possible misorientation evolution under irradiation. The section introduces and discusses the concept of in-service-induced damage as an irradiation-assisted stress-corrosion cracking precursor. Section 5 summarizes the work performed. As expected, the present work results are beneficial for exploring and understanding degradation mechanisms in highly irradiated in-core materials found in light water reactors after long-term in-service life.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Effect of laser scanning speed on the microstructure, phase transformation and mechanical property of NiTi alloys fabricated by $\mathrm{LPBF}$

This study investigated the effects of laser scanning speed on the microstructure, phase transformation and properties of NiTi alloys fabricated by laser powder bed fusion (LPBF). In this study, the contributions of metallurgical factors under different scanning speeds, such as Ni evaporation, Ni4Ti3 precipitation, dislocations and internal stress, to the transformation temperature and transformation latent heat were clarified through specially designed experiments. Ni evaporation is found to have the most profound effect, followed by precipitation. Increasing scanning speed is found to reduce Ni loss, thus cause less increase in the transformation temperature and transformation heat of the LPBF-NiTi alloys. Increasing scanning speed also increases the microstructure non-uniformity and thus widens the transformation temperature interval. The orientations of residual stress exhibit strong crystallographic stiffness dependence. The LPBF-NiTi alloys with different scanning speeds all exhibited high strains (>13.4%) and excellent shape memory effect. A LPBF-NiTi honeycomb structure exhibited 96% shape recovery rate after a 60% pre-compressive deformation. Besides, there is an optimum scanning speed for minimum porosity and smallest average pore size. However, the pore structure is found to have weak influence on the tensile behaviour of the LPBF-NiTi alloys, possibly due to the high defect tolerance of the martensitic transformation.

36 MATERIALS SCIENCE↗

Orientation dependence of the effect of short-range ordering on the plastic deformation of a medium entropy alloy

Multi-principal-element alloys (also known as medium and high entropy alloys) offer a much larger and richer design space than conventional alloys, providing opportunities for discovering new functionalities and their governing physics. Some of these alloys exhibit an outstanding combination of high strength and ductility, linked to the activation of various deformation modes triggered by low-energy stacking faults. However, a pressing question remains: Is the plasticity of medium- and high-entropy alloys governed only by stacking fault energy, or does atomic short-range order (SRO) play a role? Here, to answer this, we investigated how SRO affects the deformation in single-crystalline NiCoCr, with previous contradictory findings. First, we established unique experimental evidence for SRO formation in bulk single crystals using high-energy synchrotron transmission X-Ray Diffraction. By tuning the degree of SRO by aging at high temperatures, twinning density and strain-induced martensitic phase transformation can be significantly increased in the [110] and [111] orientations under tension, increasing the tensile ductility; yet, no increase was observed along the [001] orientation due to lack of TWinning-Induced Plasticity (TWIP) or TRansformation-Induced Plasticity (TRIP), indicating a strong crystallographic orientation dependence. Our first-principles thermodynamic calculations unequivocally show SRO exists and governs the observed microstructural evolution and deformation hardening behavior. Here we find direct proof that SRO triggers a simultaneous TWIP and TRIP in NiCoCr, a rare microstructural evolution path. Our findings establish that the interplay of SRO and plasticity could be exploited to alter deformation modes and yield unprecedented mechanical response in medium- and high-entropy alloys.

36 MATERIALS SCIENCE↗

Impact of Backbone Rigidity on the Thermomechanical Properties of Semiconducting Polymers with Conjugation Break Spacers

There remains a lack of fundamental understanding in theroleofbackbonerigidityonthe thermomechanical properties of conjugated polymers. Here, we provide the first holistic approach to understand the fundamental influence of backbone rigidity on an n-type naphthalene diimide-based conjugated polymer, denoted by PNDI-Cx, through insertion of a flexible conjugation break spacer (CBS). CBS lengths are varied from fully conjugated with zero alkyl spacer (PNDI-C0) to a seven- carbon alkyl spacer (PNDI-C 7 ), with the CBS engineered into each repeat unit for systematic evaluation. Solution small-angle neutron scattering and oscillatory shear rheometry were employed to provide the first quantitative evidence of CBS influence over conjugated polymer chain rigidity and entanglement molecular weight (M e ), demonstrating a reduction in the Kuhn length from 521 to 36 Å for fully conjugated PNDI-C0 and PNDI-C6, respectively, as well as a nearly consistent Me of ~15 kDa upon the addition of CBS. Thermomechanical properties, such as elastic modulus and glass-transition temperature, were shown to decrease with an increasing length of CBS. An extraordinary ductility, upwards of 400% tensile strain before fracture, was observed for high-molecular-weight PNDI-C4, which we attribute to a high number of entanglements and disruption of crystallization. Furthermore, the deformation mechanism for PNDI-Cx was studied under strain through X-ray diffraction, polarized UV-vis spectroscopy, and atomic force microscopy. Overall, this work sheds light on the important role of backbone rigidity in designing flexible and stretchable conjugated polymers.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗