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At least 235 records · Page 13

The roles of kinematic constraint and diffusion in non-equilibrium solid state phase transformations of Ti-6Al-4V

A solid state phase transformation of Ti-6Al-4V was studied using high speed in situ x-ray diffraction measurements made during rapid cooling of a cold metal transfer arc weld bead deposited onto a water cooled substrate. Analysis of body centered cubic (BCC) and hexagonal close packed (HCP) lattices revealed an abrupt, nonlinear shift in the lattice parameters of both phases just after the HCP phase had nucleated. Postmortem transmission electron microscopy confirmed that V diffusion was mostly suppressed during cooling. Together, these results indicate that at this cooling rate of approximately 10 4 K/s, which is representative of cooling rates of many additive manufacturing and welding processes, kinematic coherency of the BCC–HCP interfaces gives rise to the anomalous lattice expansion and contraction behaviors of both phases during the initial nucleation and growth stages of (mostly) martensitic transformation from BCC to HCP; the role of diffusion in such lattice anomalies is shown to be minimal.

36 MATERIALS SCIENCE↗

Metal additively manufactured wavy fin cold-plate architecture for improved thermal-hydraulic performance

Rapid growth in artificial intelligence and data center workloads demands high-performance liquid cooling to manage increasing chip power. This study presents two metal-additive-manufactured cold plates with sinusoidal fins, constant-amplitude wavy fins and linearly variable-amplitude wavy fins and compares them against metal-additive-manufactured straight fins using experiments conducted at 1 kW heat dissipation as well as high-fidelity 3D conjugate computational fluid dynamic simulations. The cold plates were printed in AlSi10Mg material and underwent design using a Python-automated workflow prior to manufacture and testing. The experiments show that wavy fins reduce the normalized thermal resistance by 35 to 45 % at water flow rates from 1 to 4 LPM. At a fixed 20 kPa pressure drop, the variable-waviness design lowered peak surface temperature by 9 °C and thermal resistance by 51 %, while edge-channel maldistribution in the constant wavy fin design limited gains. A thermal resistance breakdown revealed that 55–63 % of the total thermal resistance in wavy designs comes from base heat conduction, 27–33 % from fin heat conduction, and 9–13 % from fin heat convection, indicating the need to address conduction bottlenecks. Parametric sweeps identify a 3 mm fin pitch as optimal, and that horizontal inlet/outlet manifolds further reduce pressure drop by 30–60 % and thermal resistance by 9–16 % relative to vertical inlet-outlet manifolds. The results yield comprehensive guidelines for fin geometry, manifold alignment, material selection and additive-manufacturing constraints to realize high-performance liquid-cooled cold plates for power-dense electronics.

3d printing↗

Advanced manufacturing provides tailor-made solutions for crystallography with x-ray free-electron lasers

Serial crystallography at large facilities, such as x-ray free-electron lasers and synchrotrons, evolved as a powerful method for the high-resolution structural investigation of proteins that are critical for human health, thus advancing drug discovery and novel therapies. However, a critical barrier to successful serial crystallography experiments lies in the efficient handling of the protein microcrystals and solutions at microscales. Microfluidics are the obvious approach for any high-throughput, nano-to-microliter sample handling, that also requires design flexibility and rapid prototyping to deal with the variable shapes, sizes, and density of crystals. Here, we discuss recent advances in polymer 3D printing for microfluidics-based serial crystallography research and present a demonstration of emerging, large-scale, nano-3D printing approaches leading into the future of 3D sample environment and delivery device fabrication from liquid jet gas-dynamic virtual nozzles devices to fixed-target sample environment technology.

36 MATERIALS SCIENCE↗

Degradation science: Integrating modeling and experiments to predict localized corrosion processes (Annual Progress Report)

Additively manufactured (AM) eutectic high-entropy alloys (EHEAs), such as nano-lamellar AlCoCrFeNi 2.1 , have excellent strength, ductility, and wear resistance even at elevated temperatures, but their corrosion behavior in aggressive acids at different length scales remain poorly understood. This work investigates the corrosion behavior of laser powder bed–fused (L-PBF) AlCoCrFeNi 2.1 as a function of annealing temperatures, probing degradation mechanisms from nanoscopic to macroscopic length scales. The alloy is dual phase consisting of a ductile FCC L1 2 phase and a high-strength BCC B2 phase. Rapid solidification during L-PBF produces a far-from-equilibrium nano-lamellar structure with nearly homogeneous elemental distribution, which tends to evolve upon annealing toward Cr/Co/Fe-enriched FCC and Al/Ni-enriched B2. Three conditions were studied: as-printed, 600 °C/5 h, and 1000 °C/1 h, over which B2 lamellae coarsen, lamellar spacing increases, and elemental segregation becomes more prominent. Microstructure and chemistry were characterized by scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS), while in-situ electrochemical atomic force microscopy (EC-AFM) was used to link early (<5 h) local dissolution to microstructure after exposure in sulfuric acid. EC-AFM highlights preferential dissolution of the BCC/B2 phase where the surrounding matrix is Cr-depleted and directly quantifies the dissolution rates within individual phases, tracks the transition from early nano-scale attack to partial repassivation, to correlate height differences with current and impedance responses. To monitor longer-term behavior (up to 96 h), ex-situ AFM, SEM, and confocal imaging were combined with conventional bulk electrochemical tests, bridging nanoscale observations to micro/meso-scale damage morphologies. At the meso-scale, the deepest dissolution channels align with the build-direction lamellae and melt-pool boundaries, indicating that printing directionality guides the propagation of these localized corrosion sites. Annealing modifies corrosion by restructuring BCC/FCC phase fractions, lamellar spacing, and Cr/Al segregation, thereby changing the cathode/anode ratio and passive film stability. The results clarify how as-printed and annealed nano-lamellar architectures differ in their susceptibility to selective dissolution; how elemental segregation competes with residual stresses along the build direction. With these insights, future work will use CALPHAD-guided alloy modification to stabilize higher Cr contents in the B2 phase while retaining a dominant FCC+B2/BCC microstructure, with the goal of designing mechanically robust, corrosion-resistant EHEAs for safety-critical applications to leverage the LLNL’s broader national and global security mission.

36 MATERIALS SCIENCE↗

Post-build stress-relief optimization for laser powder bed fusion 316H stainless steel

Nuclear energy remains a critical component of a diversified and efficient energy portfolio, offering reliable, high-capacity, and low-carbon power. However, in the U.S., aging infrastructure and the slow qualification and deployment of advanced materials and manufacturing techniques hinder progress in next-generation reactor technologies. This study explores the application of laser powder bed fusion (LPBF) additive manufacturing for stainless steel 316H, with a focus on optimizing post-build heat treatments to enhance material properties for high-temperature nuclear applications. The research targets the optimization of stress-relief temperatures to alleviate postbuild residual stresses, ensuring improvements in the microstructural corelated properties. A series of microstructural and mechanical evaluations were performed on LPBF-printed SS-316H samples which were subjected to annealing at temperatures varying between 650 °C and 850 °C. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy analyses revealed that increasing the heattreatment temperature accelerated dislocation recovery. Vickers microhardness measurements showed an initial reduction in values, followed by stabilization over extended durations at all the temperatures. While higher temperatures facilitated faster recovery, they also promoted carbide precipitation along grain and solidification cell boundaries, narrowing the safe processing window. In contrast, heat treatment at 650°C preserved the cellular substructure and enabled controlled carbide precipitation over time. In conclusion, these findings highlight the importance of time–temperature optimization and suggest that 650°C for up to 2 h provides the most favorable balance between recovery and carbide control for a stress-relief treatment.

316 stainless steel↗

Adhesion of Self-Complementary, Sinusoidal Surfaces Fabricated Using Two-Photon Polymerization

Microscale, pick-and-place assembly is a non-lithographic assembly method poised to impact diverse fields including flexible electronics, microfluidics and robotics. However, a major technological challenge is the need to deterministically control adhesion between parts. Here, switchable adhesion involving 3D-printed, self-complementary surfaces is demonstrated. Mechanical properties of metasurfaces pressed against flat, rigid substrates are modeled using finite element methods. A series of flat slabs and metastructured slabs with 2D sinusoidal surfaces are printed using two-photon polymerization (2PP) of a shape-memory resin. The surface frequency of featured slabs was varied between $3.\bar3$ mm −1 and $26.\bar6$ mm −1 with similar amplitudes. Adhesion between printed metasurfaces and glass and between printed, self-complementary metasurfaces is studied above and below the cured resin’s glass transition temperature (∼45 °C). Simple heating of adhering surfaces to above 60 °C lowers adhesion, and compression of surfaces while above the glass transition temperature followed by cooling to room temperature elevates adhesion. The nominal adhesive strength between printed, self-complementary surfaces, as determined by the maximum observable pull-off stress, exceeds 3 MPa. Further tailoring complementary surfaces for adhesion control may facilitate microscale disassembly for recovery of components or precious metals.

amorphous materials↗

Self-contained, automated, long-term sensor system for monitoring of soil and water nutrients in fields

An automated, fieldable ion-selective sensor system for frequent detection of nutrients in soils or water is set forth. In one aspect, an integrated small form-factor housing includes a battery, processor, a fluid manipulation unit and reservoirs, and a chemical species detection cell. A flow-through sampling head can be connected to the detection cell and a waste reservoir by flexible tubing sealingly connected at opposite ends of the tube. In one aspect, improved performance of the ion-selective sensor includes adding an ion-to-electron transfer interlayer between an ion-selective membrane and its working electrode. In one aspect, the sensor is solid-state and uses printed polymeric composite of POT-MoS$_{2}$. The use of a porous tube for a sampling head and fluid connection at opposite ends allows not only fluid to be removed from the head to the detection cell for measurement but also flow in an opposite direction and out to a waste reservoir to clean and reset for a next sample measurement.

60 APPLIED LIFE SCIENCES↗

Temperature-Dependent Sheet and Contact Resistivity Measurements on Ag and Ag-Ni Circuit Pastes

The metal circuits and brazes used in electronic, energy conversion, and/or energy storage devices often have difficulty wetting and adhering to ceramic and/or ceramic-passivated metal substrates. Here, a novel Particle Interlayer Directed Wetting and Spreading (PIDWAS) technique is demonstrated that utilizes screen printing, the low wetting angle of silver on nickel, and the high work of adhesion between nickel and various ceramics to produce well-adhered, self-assembled silver patterns on ceramic and/or stainless-steel substrates not normally wet by silver. The resulting Ag-Ni circuits have higher sapphire adhesion strengths (up to 30 MPa on sapphire), higher densities (>97% on sapphire), and similar high-temperature electronic resistivities to those made using commercially-available Heraeus C8710 or DAD-87 silver circuit pastes. Similarly, Ag-Ni brazes between a variety of ceramic and/or stainless-steel substrates have better microstructural stability with rapid thermal cycling, reduction-oxidation cycling, and dual atmosphere isothermal aging than conventional Ag-CuO brazes. In addition, the residual Ni in these Ag-Ni circuits and brazes can be used to chemically getter surface segregated Al, ensuring low contact resistances on a variety of chromia- and/or alumina-passivated stainless steels. Reference: [1] Hu G, Zhou Q, Bhatlawande A, Park J, Termuhlen R, Ma Y, Bieler TR, Yu HC, Qi Y, Hogan T & Nicholas JD. Patterned Nickel Interlayers for Enhanced Silver Wetting, Spreading and Adhesion on Ceramic Substrates. Scripta Materialia, 2021; 196, 113767. 10.1016/j.scriptamat.2021.113767 [2] Park J, Phongpreecha T, Nicholas JD & Qi Y. Enhanced Liquid Metal Wetting on Oxide Surfaces via Patterned Particles. Acta Materialia, 2020; 199, 551-560. 10.1016/j.actamat.2020.08.037

Bhatlawande, Aishwarya↗

High-pressure high-temperature melting and recrystallization of nanolamellar high-entropy alloys

Additively manufactured (AM) High Entropy Alloys (HEAs) are notable for their exceptional high-yield strength and large tensile ductility. The nanolamellar Eutectic HEA (EHEA) AlCoCrFeNi 2.1 was fabricated by laser powder bed fusion (L-PBF) in the as-printed form (EHEA1) and subsequently annealed at 1000oC (EHEA2) and 600oC (EHEA3) to achieve a broad range of mechanical properties. EHEA2 and EHEA3 samples were studied using Scanning transmission electron microscopy (STEM), energy dispersive X-ray diffraction (EDXRD) at high-pressures and high temperatures, nanoindentation hardness and modulus measurements. According to EDXRD EHEA2 and EHEA3 are composed of B2 and L1 2 phases. High-pressure high-temperature EDXRD studies show melting for EHEA2 at 1698 ± 25 K at a pressure of 6.5 GPa and melting for EHEA3 at 1598 ± 25 K at a pressure of 5.8 GPa. Post-melt and recrystallized samples were recovered at ambient conditions, and XRD analysis showed retention of B2 and L1 2 phases, although a new σ phase appeared for both EHEA2 and EHEA3 samples due to high-pressure and high-temperature melting and recrystallization experiment. SEM analysis also demonstrated the preservation of the nanolamellar morphology. Nanoindentation studies revealed that recrystallized EHEAs retain their original mechanical property hierarchy, with EHEA3 being 47% harder than EHEA2, largely related to higher content of B2-phase and retention of nanolamellar morphology. We also present Pressure-Volume-Temperature (P-V-T) data for 3-D printed and annealed eutectic high entropy alloys and extract mechanical and thermal properties data.

36 MATERIALS SCIENCE↗

High-Throughput Microfluidic Electroporation (HTME): A Scalable, 384-Well Platform for Multiplexed Cell Engineering

Electroporation-mediated gene delivery is a cornerstone of synthetic biology, offering several advantages over other methods: higher efficiencies, broader applicability, and simpler sample preparation. Yet, electroporation protocols are often challenging to integrate into highly multiplexed workflows, owing to limitations in their scalability and tunability. These challenges ultimately increase the time and cost per transformation. As a result, rapidly screening genetic libraries, exploring combinatorial designs, or optimizing electroporation parameters requires extensive iterations, consuming large quantities of expensive custom-made DNA and cell lines or primary cells. To address these limitations, we have developed a High-Throughput Microfluidic Electroporation (HTME) platform that includes a 384-well electroporation plate (E-Plate) and control electronics capable of rapidly electroporating all wells in under a minute with individual control of each well. Fabricated using scalable and cost-effective printed-circuit-board (PCB) technology, the E-Plate significantly reduces consumable costs and reagent consumption by operating on nano to microliter volumes. Furthermore, individually addressable wells facilitate rapid exploration of large sets of experimental conditions to optimize electroporation for different cell types and plasmid concentrations/types. Use of the standard 384-well footprint makes the platform easily integrable into automated workflows, thereby enabling end-to-end automation. We demonstrate transformation of E. coli with pUC19 to validate the HTME's core functionality, achieving at least a single colony forming unit in more than 99% of wells and confirming the platform's ability to rapidly perform hundreds of electroporations with customizable conditions. This work highlights the HTME's potential to significantly accelerate synthetic biology Design-Build-Test-Learn (DBTL) cycles by mitigating the transformation/transfection bottleneck.

Gaillard, William R↗

Two-Phase Cooling for High Packaging Density Planar Inverter: Cooperative Research and Development Final Report, CRADA Number CRD-15-00592

The project objective was to utilize two-phase heat transfer to enable compact and power-dense inverters. The high heat transfer capacity and near isothermal characteristics of two-phase cooling can enable higher power densities, reducing the size and cost of the power electronics system. This project focused on developing efficient, passive (no pump or compressor) two-phase cooling strategies that consist of an air-cooled condenser and evaporator. This report describes the modeling work conducted to design the evaporator and air-cooled condenser for a prototype inverter development work underway in the John Deere. Prototypes of the final evaporator and condenser designs were then fabricated via 3D printing for testing. Experiments on the evaporator confirmed that this component can meet the heat load and junction temperatures requirements for Si IGBT (insulated-gate bipolar transistor) inverter. Experiments with the air-cooled condenser were not possible due to leaks through the condenser walls.

33 ADVANCED PROPULSION SYSTEMS↗

Asymmetric side-chain engineering in semiconducting polymers: a platform for greener processing and post-functionalization of organic electronics

Organic semiconducting polymers are a powerful platform for the design of next-generation technologies due to their excellent optoelectronic properties and solution processability, allowing access to low-cost and scalable manufacturing techniques such as spin-coating, slot-die coating and roll-to-roll printing. However, their extended π-conjugation results in low solubility, requiring the use of toxic halogenated solvents to generate thin films and devices. Furthermore, accessible post-functionalization of semiconductors toward the development of multifunctional devices and sensors remains a challenge due to limited solid-state chemistry for alkyl side chains. In this work, an asymmetric side-chain engineering approach was used to introduce terminal hydroxyl moieties alongside traditional solubilizing branched alkyl chains into an isoindigo-based polymer. The hydroxyl moieties led to significantly improved processability in alcohol-based solvents without sacrificing electronic performance in thin film organic field-effect transistors. Solid state morphologies of the thin films processed from both alcohol-based and traditional halogenated solvents were further characterized using atomic force microscopy and grazing incidence wide angle X-ray scattering. Additionally, Cryo-EM was utilized in order to characterize the role of asymmetric side-chain functionality in solution state aggregation. The versatility of this design was further probed using fluorescein isothiocyanate to directly functionalize the asymmetric polymer in thin film. Furthermore, this facile solid-state post-functionalization further demonstrates asymmetric side-chain engineering to be a viable approach toward the development of sustainably manufactured multifunctional electronics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Deformation Mechanism Transition in Additively Manufactured Compositionally Graded Fe-Base Alloys

Microstructure-dependent deformation and fracture behavior was investigated for an additively manufactured compositionally graded alloy (CGA) printed using the laser-directed energy deposition (L-DED) method to explore an alternative approach for dissimilar metal joints in nuclear energy systems. The electron backscatter diffraction (EBSD) maps from scanning electron microscopy (SEM) display a clear microstructural transition with decreasing austenite-forming elements (Ni and Mn), from an austenite (γ) dominant structure, to a complex composite structure containing ferrite (α), martensite (α') and retained austenite, and then to a fully ferritic structure. EBSD data were recorded in situ during tensile testing in SEM, and the evolution of the deformation mechanism and microstructure was characterized using Kikuchi diffraction pattern analysis. Complementary analysis for high-resolution features was also performed using scanning transmission electron microscopy (STEM). The Ni/Mn-rich austenite-dominant microstructures showed a complex deformation mechanism of two-step martensitic transformation (γ→ε→α'), whereas the minor austenite phase retained in the ferrite and/or martensite matrix showed a single transformation route (γ→α'). Ordinary dislocation glide and twinning via partial dislocation glide were observed in the austenite deformation. Meanwhile, the ferrite and martensite grains deformed mainly by ordinary dislocation slips and grain rotation. Furthermore, static tensile fracture was also highly dependent on local composition and phase constituents.

36 MATERIALS SCIENCE↗

Electron beam surface remelting enhanced corrosion resistance of additively manufactured Ti-6Al-4V as a potential in-situ re-finishing technique

This study explores the effect of surface re-finishing on the corrosion behavior of electron beam manufactured (EBM) Ti-G5 (Ti-6Al-4V), including the novel application of an electron beam surface remelting (EBSR) technique. Specifically, the relationship between material surface roughness and corrosion resistance was examined. Surface roughness was tested in the as-printed (AP), mechanically polished (MP), and EBSR states and compared to wrought (WR) counterparts. Electrochemical measurements were performed in chloride-containing media. It was observed that surface roughness, rather than differences in the underlying microstructure, played a more significant role in the general corrosion resistance in the environment explored here. While both MP and EBSR methods reduced surface roughness and enhanced corrosion resistance, mechanical polishing has many known limitations. The EBSR process explored herein demonstrated positive preliminary results. The surface roughness (R a ) of the EBM-AP material was considerably reduced by 82%. Additionally, the measured corrosion current density in 0.6 M NaCl for the EBSR sample is 0.05 µA cm –2 , five times less than the value obtained for the EBM-AP specimen (0.26 µA cm –2 ).

42 ENGINEERING↗

Charge regulation effects on colloidal mixture nanoparticles

Changes in pH within a system containing dissociable sites affect the protonation and deprotonation of these groups, thereby influencing their physical properties. In response, the system modifies their surface charge, affecting electrostatic interactions, aggregation, stability, and structural behavior. Although the pH can be tuned in experiments, it is difficult to model this phenomenon using simulations or theoretical approaches. Here, we perform hybrid Monte Carlo-molecular dynamics simulations to model charge regulation effects in an equimolar colloidal charged system. We compare charge regulation effects with those of a system in which the charges of colloidal nanoparticles are not dissociable. The comparison between the two cases modifies the phase diagram, and it changes the volume fraction where a percolation network of nanoparticles is found. Charge regulation is found to destroy network formation, as the charge in the nanoparticles is modified because of the cooperativity dependency of the degree of charge dissociation sites among the nanoparticles favoring cluster formation. Furthermore, our work suggests that the ionic and/or electronic conductivity in functionalized nanoparticles can be modified by changing pH values. It also guides the experimental design of oppositely charged nanoparticles as inks for 3D printing processes.

Classical statistical mechanics↗

First results from a multiplexed and massive instrument with sub-electron noise Skipper-CCDs

Here, we present a new instrument composed of a large number of sub-electron noise Skipper-CCDs operated with a two stage analog multiplexed readout scheme suitable for scaling to thousands of channels. New, thick, 1.35 Mpix sensors, from a new foundry, are glued into a Multi-Chip Module (MCM) printed circuit board on a ceramic substrate which has 16 sensors each. The instrument, that can hold up-to 16 MCMs, a total of 256 Skipper-CCD sensors (called a Super-Module with ≈ 130 grams of active mass and 346 Mpix), is part of the R&D effort of the OSCURA experiment which will have ≈ 94 super-modules. Experimental results with 10 MCMs and 160 Skipper-CCDs sensors are presented in this paper. This is already the largest ever built instrument with single electron sensitivity CCDs using nondestructive readout, both, in terms of active mass and number of channels.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗