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At least 1,009 records · Page 56

Towards underwater additive manufacturing via additive friction stir deposition

Given the challenges in feed material supply and quality control, metal additive manufacturing has rarely been implemented in austere environments, especially underwater. This paper explores the underwater operation potential of an emerging solid-state additive technology: additive friction stir deposition, wherein material feeding and bonding are enabled by mechanical forces with minimal influences from water. It is demonstrated that additive friction stir deposition of 304 stainless steel can be successfully performed with the print head and substrate immersed in water. High temperature is reached in the deposition zone (>60% melting temperature); the material deposition behavior is similar to that in typical open-air operation. The as-deposited material is fully-dense, having fewer annealing twins and a substantially smaller grain size than the feed material (4.98 μm vs. 31.44 μm ). Such microstructural changes stem from dynamic recrystallization caused by the large strain and high temperature introduced during deposition. In addition to grain refinement, small equiaxed dispersoids (~2–3 μm or less) are formed and evenly distributed in the austenite steel matrix. Rich in Cr, Mn, and O, these particles likely result from the reaction between the elements in stainless steel and water at elevated temperatures.

16 TIDAL AND WAVE POWER↗

Material Properties of Zirconium Hydride Phases in Zircaloy-4 Getter Tubes Mapped by Atomic Force Microscopy

Nickel plated Zircaloy-4 tubing (“getter tubing”) is an important functional component in Tritium Producing Burnable Absorber Rods (TBPARs). Getter tubes are used to capture tritium produced during reactor operations and convert it from a gas to a solid by reacting it with Zr to form ZrHx compounds. Previous studies (PNNL-27232, TTP-8-004, and TTP-30710) on forming Zircaloy-4 hydrides demonstrated that hydride concentration gradients formed under prototypic hydriding conditions and that the microstructure of hydrides formed at 350°C is different than those formed at 500°C, a temperature typically used by the Tritium Technology Program (TTP) for getter rate loading experiments. Differences in hydride distribution, microstructure, and phases were characterize using scanning electron microscopy methods. However, the impact of these differences on material properties is not well understood. The goal of this project was to determine whether atomic force microscopy could observe subtle differences in material properties of single domains of hydride phases formed in Zircaloy-4. These properties include surface structure, hardness, thermal conductivity, and magnetic susceptibility.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Comparison of Electron Beam and Laser Beam Powder Bed Fusion Additive Manufacturing Process for High Temperature Turbine Component Materials, Phase II. CRADA Final Report

The evolving additive manufacturing (AM) technology is now at the point where some metallic turbine components are being fabricated for both development and production purposes. The goal of this phase II project is to continue the evaluation of AM Nickel Alloy X fabricated by electron beam (EB) or laser beam (LB) powder bed fusion (PBF) process for gas turbine applications. Microstructure, mechanical and oxidation properties characterization was conducted on test specimens produced with powders of different chemistries within the typical material specification range. Powders with high Silicon (Si) content for the LB-PBF and low Si content for the EB-PBF displayed significant cracking levels in the AM Nickel Alloy X material. Accordingly, optimum fatigue performance would require careful control of powder chemistry, optimization of the fabrication parameters for a given powder and use of hot isostatic pressing (HIP) post treatment. Oxidation testing conducted at 1472°F (800ºC) in air showed that the roughness of the EB-PBF specimens led to an increase in specimen mass change, but overall the AM specimens exhibited oxidation behavior at 1472°F (800ºC) that is appropriate for applications in gas turbine engines. Assessment of the geometric capability of the LB-PBF and EBPBF systems using artifacts representative of turbine component geometries revealed that the LB-PBF process is well-suited for the fabrication of intricate geometries needed for turbine engine fuel injector components, but further process development is required to improve the EB-PBF system feature resolution.

36 MATERIALS SCIENCE↗

A REDUCED ORDER MODELING APPROACH TO PROBABILISTIC CREEP-DAMAGE PREDICTIONS IN FINITE ELEMENT ANALYSIS

This paper introduces a computationally efficient Reduced Order Modeling (ROM) approach for the probabilistic prediction of creep-damage failure. Component-level probabilistic simulations are needed to assess the reliability and safety of high-temperature components. Full-scale probabilistic creep-damage modeling in finite element (FE) approach is computationally expensive requiring many hundreds of simulations to replicate the uncertainty of component failure. To that end, ROM is proposed to minimize the elevated computational cost while controlling the loss of accuracy. It is proposed that full-scale probabilistic simulations can be completed in 1D at a reduced cost, the extremum conditions extracted, and those conditions applied for lower-cost 2D/3D probabilistic simulations of components that capture the mean and uncertainty of failure. The probabilistic Sine-hyperbolic (Sinh) model is selected which in previous work was calibrated to alloy 304 stainless steel. The Sinh model includes probability density functions (pdfs) for test condition (stress and temperature), initial damage (i.e. microstructure), and material properties uncertainty. The Sinh model is programmed into ANSYS finite element software using the USERCREEP.F material subroutine. First, the Sinh model and FE code are subject to verification and validation to ensure the accuracy of the simulations. Numerous Monte Carlo simulations are executed in a 1D model to generate probabilistic creep deformation, damage, and rupture data. This data is analyzed and the probabilistic parameters corresponding to extreme creep response are extracted. The ROM concept is applied where only the extreme conditions are applied in the 2D probabilistic prediction of a component. The probabilistic predictions between the 1D and 2D geometry is compared to assess ROM for creep. The accuracy of the probabilistic prediction employing the ROM approach will potentially reduce the time and cost of simulating complex engineering systems. Future studies will introduce multi-stage Sinh, stochasticity, and spatial uncertainty for improved prediction.

36 MATERIALS SCIENCE↗

Structural Heterogeneity in Medium-Entropy AgMnSbPbTe 4 for Glassy Thermal Transport and High Thermoelectric Performance

Medium-entropy semiconductors represent a unique category of entropy-engineered materials. They possess a considerable level of randomness in atomic mixing, although this is not sufficient to conclusively achieve single-phase structure stabilization, in contrast to high-entropy materials. This introduces strong competition between the formation of different phases, which can potentially lead to structural heterogeneity. Here, in this work, we uncover endotaxial nanoprecipitates in the microscopically identified homogeneous medium-entropy semiconductor AgMnSbPbTe 4 . These nanoprecipitates initially crystallize in a cubic phase $(Fm\bar{3}m)$ within kinetically stabilized AgMnSbPbTe 4 , subsequently evolving into a thermodynamically stable monoclinic phase $(P2_1/c)$ during thermal annealing while maintaining an endotaxial relationship with the matrix lattice. This nanophase segregation and the resultant lattice mismatch at interfaces introduce strain fluctuations up to 5% at intervals of 20 nm across the entire microstructure. Within the matrix phase, atomic displacement of up to 23 pm was observed. This structural heterogeneity results in glass-like thermal transport behavior, achieving an ultralow lattice thermal conductivity κ L = 0.312 Wm –1 K –1 at 800 K, which is in accordance with the amorphous limit predicted by the Cahill model. The synergy of band convergence effect and well-maintained carrier mobility leads to a maximum ZT of 1.72 at 800 K and an average ZT avg of 1.02 over the temperature range of 300–825 K. This study highlights that the underexplored structural heterogeneity in medium-entropy semiconductors can potentially yield beneficial phenomena, such as the phonon-glass electron-crystal transport behavior in this case, which holds promise for advancing thermoelectric applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Shape memory behavior and recovery force of 4D printed textile functional composites

Four-dimensional (4D) printing of multi-directionally reinforced preforms has tremendous potential for the development of next generation functional composites by using the capabilities of 3D printing technology, 3D textile preform design, and polymer shape memory behavior. This paper demonstrates the shape memory behavior and recovery force of 4D printed circular braided tube preforms and their silicone elastomer matrix composites. The preforms were printed by fused deposition modeling using the shape memory polymer (SMP), polylactic acid (PLA). The effects of braiding angle, tube wall thickness, and shape recovery temperature on the shape memory behavior of 4D printed tube preforms and their silicone elastomer matrix composites have been characterized. Measurements of shape recovery forces of the preform and composite were conducted using dynamic mechanical analysis (DMA). The braided microstructural parameters and shape recovery temperature have a significant effect on the preform shape memory behavior. The introduction of the silicone elastomer matrix greatly enhances the shape recovery force, shape recovery ratio, as well as radial compressive failure load of the 4D printed preform/silicone elastomer matrix composite. Finally, building on these results, a potential application for 4D printed textile functional composites is presented.

42 ENGINEERING↗

Intrinsic size dependent plasticity in BCC micro-pillars under uniaxial tension and pure torsion

The mechanical behavior of submicron body-centered cubic (BCC) micro-pillars is investigated by three-dimensional dislocation dynamics (DD) simulations to better understand the governing mechanisms for size dependent plasticity under uniaxial tension and pure torsion. A formula is developed to compute the incremental plastic twist due to dislocation motion in DD simulations. The DD simulations show that different dislocation microstructures are created depending on the loading conditions, which leads to different size dependent mechanical behavior. While in tension plasticity is mainly governed by the kinetics of dislocation motion controlled partly by the surface dislocation sources, plastic flow in torsion is controlled by dislocation pile-ups associated with strain gradients. The simulation results also reveal a Bauschinger effect and plastic recovery under cyclic twist, which have been observed in recent experiments.

36 MATERIALS SCIENCE↗

Imaging electric field dynamics with graphene optoelectronics

The use of electric fields for signalling and control in liquids is widespread, spanning bioelectric activity in cells to electrical manipulation of microstructures in lab-on-a-chip devices. However, an appropriate tool to resolve the spatio-temporal distribution of electric fields over a large dynamic range has yet to be developed. Here we present a label-free method to image local electric fields in real time and under ambient conditions. Our technique combines the unique gate-variable optical transitions of graphene with a critically coupled planar waveguide platform that enables highly sensitive detection of local electric fields with a voltage sensitivity of a few microvolts, a spatial resolution of tens of micrometres and a frequency response over tens of kilohertz. Our imaging platform enables parallel detection of electric fields over a large field of view and can be tailored to broad applications spanning lab-on-a-chip device engineering to analysis of bioelectric phenomena.

59 BASIC BIOLOGICAL SCIENCES↗

Characterization and Modeling of Deformation Induced Damage in Titanium Alloys

Over the lifetime of their DOE support, and specifically during the past funding cycle, the PIs have primarily focused on ambient temperature studies of the mechanisms of heterogeneous deformation and shear transfer at GBs. The PIs have developed and applied a broad array of experimental approaches complemented by advanced computational methods and simulations to enable new understanding of GB shear transfer, and a new approach for modeling this behavior at the mechanistic level has been established. The PIs have examined how slip behavior differs on the surface and interior of polycrystals using a variety of approaches. Some of the associated data has been used to generate 3-D models of experimentally-characterized microstructures that both support interpretation of deformation mechanisms as well as reveal where modeling needs to be improved to more closely agree with what is experimentally observed. The PIs progress in constitutive modeling of crystal plasticity has introduced explicit GB resistance to shear that depends on the mutual geometry of active slip systems. This past work places the PIs in a good position to take on the challenges associated with mechanistically understanding the interplay between GBS and slip interactions.

42 ENGINEERING↗

Elevated-temperature cyclic properties of advanced manufactured materials

Microreactor developers at the 2019 GAIN Microreactors workshop expressed a need for advanced manufacturing to fabricate microreactor components. Powder metallurgy (PM) hot isostatic pressing (HIP) is more mature than other advanced manufacturing techniques for the following reasons: 1. a code case exists for Section III, Division 1, Subsection NB components of light water reactors to be manufactured using PM HIP Alloy 316L, and 2. tensile and creep properties have been shown to be equivalent to wrought material for Type 316 stainless steel and Grade 91. Thus, PM HIP is more readily deployable in the near term. Elevated-temperature cyclic properties of PM-HIP materials, however, have not been established. The scope of testing for Code qualification could be significantly reduced compared to a new material for the following reasons: 1. only a limited amount of time consuming creep testing would be required, and 2. testing of fatigue and creep-fatigue behavior could be reduced if it can be demonstrated that the properties are comparable to wrought material. The objective of this work package is to develop an understanding of the relationship of advanced materials processing on the material characteristics as they relate to elevated-temperature component design and construction. This will be achieved by the following: • Elevated-temperature fatigue and creep-fatigue testing of PM HIP and wrought Alloy 316L. • Fracture and microstructural characterization of the PM HIP and wrought Alloy 316L. • Analysis of the elevated-temperature fatigue and creep-fatigue properties of PM HIP Alloy 316L. • Draft a report evaluating the elevated-temperature fatigue and creep-fatigue properties of PM HIP Alloy 316L. • Pursue procurement of Alloy 316H and Grade 91 manufactured using PM HIP. • Initiate scoping studies of the procured Alloy 316H or Grade 91 manufactured using PM HIP contingent upon successful material procurement.

36 MATERIALS SCIENCE↗

Effects of ternary alloy additions on the microstructure of highly immiscible Cu alloys subjected to severe plastic deformation: An evaluation of the effective temperature model

Phase evolution in dilute, strongly immiscible Cu-Mo, Cu-Mo-Ni, and Cu-Mo-Ag alloys during severe plastic deformation at low-temperature has been experimentally investigated. For the Cu95Mo05 alloy, Mo nanoparticles are formed, ~10 nm in diameter, as part of a steady state microstructure, with less than ~1 at.% Mo dissolved in the matrix. Addition of 10 or 20 at.% Ni to this binary alloy results in a significant increase in the Mo solubility, whereas comparable additions of Ag has a corresponding little effect. The steady state microstructures of alloys during ball milling of elemental powders are very similar to those during HPT processing of initially homogeneous solutions. The results are discussed in terms of an effective temperature model. Model MD simulations are presented to help relate the predictions of the effective temperature model to atomistic mechanisms.

36 MATERIALS SCIENCE↗

Novel Fabrication of a TiB{sub 2} Grain Refiner and its Effect on Reducing Hot Tearing in AZ91D Magnesium Alloy

Despite the increased use of magnesium (Mg) alloys in diverse engineering applications in recent years, further incorporation of complex Mg alloy castings remains challenging due to the alloy’s relatively high susceptibility to hot tearing. A significant reduction in hot tearing via grain refinement was achieved in aluminum and ferrous alloys; however, an effective, long-lasting and inexpensive grain refiner for aluminum-containing Mg alloys remains elusive. In this work, a TiB{sub 2} grain refiner was fabricated via a novel spark plasma sintering (SPS) powder metallurgy process. Then, its effectiveness in grain refining an AZ91D magnesium alloy was compared to that of a commercially available TiB{sub 2} grain refiner produced by hot extrusion. Due to the homogeneous distribution of the TiAl{sub 3} and TiB{sub 2} particles in the grain refiner, as well as their effect on the alloy’s microstructure evolution and solidification behavior, the SPS-TiB{sub 2} grain refiner was observed to achieve a significant reduction in the grain size and hot tearing of the Al-containing AZ91D magnesium alloy.

36 MATERIALS SCIENCE↗

Circularity in Sequence-Controlled Copolyamides Enabled by Regioselective Enzymatic Hydrolysis

Sequence-controlled polymers enable precise control over macromolecular structures and function, but both their synthesis and end-of-life management remain fundamental challenges. Achieving high sequence fidelity is synthetically demanding, and conventional depolymerization methods lack regioselectivity, leading to irreversible loss of encoded molecular information and limiting polymer circularity. Enzymatic catalysis offers a potential solution by combining substrate specificity with selective bond cleavage. Here, we report the synthesis, characterization, and regioselective enzymatic depolymerization of poly- (X,AMA), a sequence-controlled copolyamide composed of alternating hexamethylenediamine−adipic acid (MA) and pxylylenediamine− adipic acid (XA) repeat units. Poly(X,AMA) was synthesized via solid-state polycondensation (SSP) of sequence-defined oligomers, enabling precise control over repeat-unit order. Polymer microstructure and sequence fidelity were confirmed by 13 C NMR spectroscopy and MALDI−TOF mass spectrometry. Comparison with a statistical copolymer analogue and Nylon-66 demonstrated pronounced differences in crystallinity, morphology, and thermal behavior arising from sequence control. Screening of 96 Nylon hydrolase homologues against poly(X,AMA) revealed strongly enzyme-dependent depolymerization profiles. While tetrad formation was generally favored, enzymes displayed pronounced sequence selectivity, preferentially releasing distinct sequence-defined tetrads XAMA or MAXA. SSP of sequence-defined tetrad MAXA produced a copolyamide with near identical monomer ordering as poly(X,AMA). Computational modeling of enzyme−substrate complexes identified structural features consistent with the observed regioselectivity. Together, these results establish selective enzymatic depolymerization as a viable strategy for the circular recycling of sequence-controlled polymers and provide a foundation for the rational engineering of enzymes for programmable polymer deconstruction.

Amides↗

Effect of subfreezing testing temperature on tensile mechanical behavior of fine-grained magnesium

Here, the effect of testing temperature on mechanical properties and deformation mechanisms was investigated by tensile testing of fine-grained magnesium samples under a range of temperatures (i.e. room temperature 20°C, subfreezing temperatures 0°C, -30°C, and - 60°C) and microstructural observations of both untested and tested samples using electron backscatter diffraction. The results suggest that mechanical properties and deformation mechanisms were significantly affected by lowering testing temperature. Strength increased linearly and ductility decreased linearly with the decrease of testing temperature. Although twinning is generally known to be athermal, this experimental study shows that tensile twinning is the dominating deformation mechanism at room temperature, and that twinning is negligible and dislocation operation is the primary deformation mechanism at 0°C, -30°C, and -60°C

36 MATERIALS SCIENCE↗

Constitutive behavior and processing maps of a new wrought magnesium alloy ZE20 (Mg-2Zn-0.2Ce)

ZE20 (Mg-2Zn-0.2Ce) 2 is a new wrought magnesium alloy with improved extrudability and mechanical properties [1]. To understand the constitutive behavior and workability of this new alloy, Gleeble thermomechanical testing has been carried out in this study. The flow stress behavior of ZE20 was investigated between 250 °C–450 °C and 10 –3 s –1 –1.0 s –1 in isothermal compression. Constitutive descriptions of the flow stress are provided. A new general approach at application of the extended Ludwik equation is demonstrated and was found to be more accurate than the hyperbolic sine Arrhenius model while having a similar number of model constants. Processing maps were developed based on the experimental results and are verified with microstructural investigation. A region of safe processing with non-basal texture and high activity of dynamic recrystallization (DRX) was found between 375 °C and 450 °C, from 10 –1 s –1 to 10–2.5 s –1 . A region of potentially safe processing with annealing that is associated with shear band nucleation of non-basal grains was identified for temperatures as low as 300 °C and rates as high as 10 –1 s –1 .

36 MATERIALS SCIENCE↗

Quantitative Nanoscale 3D Imaging of Intergranular Corrosion of 304 Stainless Steel Using Hard X-Ray Nanoprobe

Multi-modal imaging, which visualizes changes in the structure and chemistry of the same region of interest in materials by combining various techniques, is becoming attractive to material scientists. Here, we describe a multi-modal approach to investigate intergranular (IG) corrosion of sensitized stainless steels using synchrotron-based nanoscale X-ray imaging with sensitivity to microstructure and chemical composition. Three-dimensional tomography of 304 stainless steel samples deteriorated by IG corrosion, was carried out using X-ray fluorescence and differential phase contrast imaging. These findings were further supported with surface imaging and chemical analysis using scanning electron microscopy and energy dispersive X-ray spectroscopy. The combined quantitative structural and chemical analysis indicates that chromium segregates along grain boundaries, cracking is due to IG corrosion, and Cr-enrichment occurs on the cracked surfaces. Such quantitative 3D imaging of Cr 23 C 6 nucleation at grain boundaries and Cr enriched oxides at cracked surfaces is a powerful tool to correlate IG corrosion mechanisms at nanoscale with buried grain boundary structure and alloy composition. Such understanding of IG corrosion mechanisms is critical for both the development of predictive multiscale corrosion models, and the engineering of corrosion resistant materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Role of Si substitution in modulating the coercivity and magnetic anisotropy in Fe3CoB2 nanocrystallites

In this work, we report the impact of Si substitution on the structural and magnetic properties of Fe3CoB2 nanocrystallites as a rare-earth-free hard-magnet candidate. X-ray diffraction confirmed the formation of the tetragonal phase with an average crystallite size of ∼40 nm, while the transmission electron microscopy image revealed nanosized crystallites embedded in an amorphous matrix. Room-temperature Mössbauer spectra exhibited two sextets and two doublets, indicating magnetically ordered Fe sites in the tetragonal phase along with high-spin paramagnetic FeIII species in disordered regions. ZFC–FC magnetization curves displayed field-dependent blocking behavior, consistent with paramagnetic Fe species. Singular point detection measurements revealed a high anisotropy field of ∼10.7 kOe in the pristine Fe3CoB2, and systematically decreased with Si substitution. Magnetization measurements revealed a monotonic decrease in saturation magnetization with Si content, while coercivity was observed to increase, likely due to microstructural refinement. These results establish Fe3CoB2 as a rare-earth-free material with strong magnetic anisotropy, ideal for hard magnets.

Abbas, Hur [Department of Physics, University of T↗