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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 613 records · Page 34

Design and Fabrication of a Temperature-Controlled Fueled Molten Salt Capsule Irradiation Experiment

Idaho National Laboratory (INL) is developing a Molten salt Research Temperature-controlled Irradiation (MRTI) experimental capsule for the Neutron Radiography (NRAD) reactor. The experiment is envisaged to be versatile and able to host a variety of salt-wall material combinations. The first test is designed to contain actinide-bearing chloride salt, which previously has not been subjected to a neutron field. The main objectives of the experiment are to produce irradiated salt samples for Post Irradiation Examination (PIE), to evaluate salt behavior under irradiation, and to test in-situ sensors/instrumentation. The final design for the experiment completed in 2022, and fabrication of the experiment is underway. The salt is double encapsulated providing insulation and redundancy in the case of leakage. A gas-gap between the inner capsule and the outer container enables tuning of thermal conduction to the NRAD coolant by altering its thickness and its gas-mixture. An inert gas mixture ratio in the gas-gap ensures the configurations reached a targeted average salt temperature of 600oC, while avoiding salt freezing or exceeding material limits. A resistive heater placed within a thermowell and controls the temperature of the experiment (both when the reactor is on or off). The selected configurations can contain over 10 cm3 of fuel-bearing chloride salt, which is sufficient for the purposes of the post-irradiation examination (PIE) and provides sufficient volume for two submerged thermocouple probes to monitor salt temperature. The capsule wall material is Inconel 625, and weld qualifications for the assembly have been developed. A glove-box laser weld technique was refined as part of this process to ensure a leak-tight assembly for the salt-bearing assembly and reduce the risks of impurities permeating into the salt. This work was supported through the INL Laboratory Directed Research & Development (LDRD) Program under DOE Idaho Operations Office Contract DE-AC07-05ID14517.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Femto-second Laser’s Enabling New Length Scale Fabrications for Rapid Post Irradiation Examination of Materials: Concluding LDRD Project Poster

Mechanical testing campaigns are required to qualify materials for advanced reactor conditions, yet economical and safety limitations restrict the number of standardized mechanical tests that can be performed. Reducing the size of the sample is one approach to addressing these challenges and to accelerating testing. Previous research has shown that smaller mechanical test samples produce higher yield and ultimate stress values compared to values measured from standard sample sizes: the “smaller is stronger” effect. Specimens used in accelerated material testing campaigns must reflect bulk material performance to enable engineering scale material property measurement. The objective of this research project was to determine if engineering scale mechanical behavior—the yield stress—could be measured with micro-tensile test samples smaller than traditional standard testing geometries. The relationship between yield stress and sample size was explored with two different nuclear-relevant structural materials: Zircaloy-4 and tungsten. Mechanical testing of both metals demonstrated decreasing yield stress values with increasing sample gauge size across three different sizes. Yield stress values from the largest gauge size, fabricated with a femto-second laser ablation system, approach bulk material yield stress values reported in published literature. Preliminary analysis of the tungsten samples indicates the yield stress value depends on the grain characteristics within the gauge section, in addition to the gauge size. Accompanying modeling efforts, including response surface generation and crystal plasticity approaches, further demonstrated that the size of the sample gauge section alone cannot explain the change in yield stress values.

36 MATERIALS SCIENCE↗

Method and apparatus for fabricating a hybrid tube

An apparatus for fabricating a hybrid tube includes a rotatable mandrel and a first housing configured to translate alongside the rotatable mandrel while dispensing a first strip to be helically wound about the mandrel. The first housing includes an angle adjustment mechanism to control a dispensation angle of the first strip. The apparatus also includes least one energy or adhesive source for bonding overlapping strip portions on the rotatable mandrel and forming the hybrid tube. The at least one energy or adhesive source is configured for translation alongside the rotatable mandrel.

Sinha, Sanjiv↗

Fabrication and Scale-Up of Porous Polybenzimidazole (PBI) Supports for Gas Separation Composite Membranes

Industrial gas separation often uses thin film composite (TFC) membranes comprising a porous support overlaid with a single-/multi-layer gas-selective thin film. An optimal porous support should possess high surface porosity to minimize gas transport resistance and nano-sized pores to ease pore penetration occurring during the thin film coating process. Good chemical and thermal stabilities are essential to withstand the aggressive solvents and heat required for the thin film coating and curing. However, few porous membranes satisfy all these requirements. This study presents a scalable membrane formation method of making highly porous polybenzimidazole (PBI) supports via non-solvent induced phase separation. This presentation also details the scale-up fabrication of PBI supports using a custom roll-to-roll membrane casting machine.

gas separation↗

Fabrication and characterization of nanoscale magnesium diboride and tetraboride for propulsion and hydrogen storage applications

Abstract: Boron-loaded propellants have the potential to dramatically increase the performance of solid fuel ramjets, ducted rockets, and hybrid rocket engines. However, difficult ignition of boron decreases the combustion efficiency of these propellants. One approach to solving this problem involves the use of magnesium diboride, MgB2, which ignites easier than boron. Magnesium tetraboride, MgB4, potentially offers greater energetic performance as B has a higher energy density than Mg. However, the effect of the higher boron/metal ratio on the ignition and combustion is unclear. Nanoscale MgB2 particles and quasi 2D structures are promising propellant ingredients, but the oxidation and combustion properties of nanoscale MgB4 remain unknown. Nanoscale magnesium borides are also of interest as precursors for the synthesis of magnesium borohydride, Mg(BH4)2, a promising hydrogen storage material, but hydrogenation of MgB4 has not been studied yet. The objectives of the present work included synthesis, purification, and high-energy ball milling of MgB2 and MgB4 powders as well as investigation of their hydrogen uptake, thermal decomposition, oxidation, and combustion. The powders were fabricated by combustion synthesis and by heating in a tube furnace. The latter method was superior in the synthesis of MgB4. Oxide impurities in the synthesized powders were removed by acid leaching. Nanoscale powders were obtained by ball-mill exfoliation. The hydrogen intake of the obtained magnesium borides was examined at 700 bar and 300 ℃ and did not reveal any advantage of MgB4 over MgB2. Their thermal decomposition and oxidation were investigated with thermogravimetric analysis (TGA), while their combustion was studied using laser ignition and high-speed video recording. TGA has confirmed prior observations of multistep decomposition of magnesium borides, where each step involves formation of a boride with a higher B/Mg ratio and evaporation of formed magnesium. The oxidation rates of the borides are much higher than that of boron at temperatures over 1200 °C for MgB2 and over 900 °C for MgB4. The burning rates of non-milled MgB₂ and MgB₄ powders were much higher than for the used submicron boron. Milling the MgB₂ and MgB₄ powders further increased their burning rates. The milled MgB4 burned 7.5 times faster than submicron boron.

Combustion of metals, Solid fuels, Propellants, Hy↗

Fabrication of the HFVMTF Double-Bath Cryostat

The High Field Vertical Magnet Test Facility (HFVMTF) at Fermilab is designed to test superconducting magnets up to 20 tons and 1.3 meters in diameter. Central to the facility is a double-bath superfluid helium cryostat reaching 1.8 K at 1.2 bar. Integrated with a 15 T superconducting dipole from LBNL, HFVMTF supports HTS cable testing for fusion applications. This paper presents the design and fabrication of the cryostat, with a focus on two complex components: the 2 K heat exchanger and the lambda plate. The heat exchanger thermally links sub-atmospheric and pressurized helium baths. The 1.4-meter lambda plate provides thermal isolation and structural support for over 20 tons under 1.3 bar pressure differential. Finite Element Analysis validated the vessel's integrity under maximum load conditions.

Bruce, R. [Fermilab] (ORCID:0000000234200612)↗

Nb3Sn Superconducting Radiofrequency Cavity Fabricated by Sputter Deposition from a Stoichiometric Target

Nb$_3$Sn is a promising coating material for superconducting radiofrequency cavities in next-generation accelerators due to its higher superconducting transition temperature (~18.3 K) and superheating field (~400 mT), offering the potential to surpass the intrinsic performance limits of bulk niobium. We developed a sputter coating technique employing a stoichiometric target to fabricate Nb$_3$Sn films on the inner surfaces of niobium cavities. A Nb$_3$Sn tube target, prepared by growing a >20 m thick Nb$_3$Sn coating on the surface of a Nb tube via a Sn vapor diffusion process, was used in a DC cylindrical magnetron sputtering system. Approximately 170 nm thick Nb-Sn films were sputter-coated onto flat Nb substrates positioned to replicate the beam tube and equator regions of a 2.6 GHz cavity, followed by annealing at 950 °C for 3 hours to form Nb$_3$Sn. The composition, morphology, and structure of the annealed Nb$_3$Sn films were examined. Then, a ~1.2 m-thick film was sputter-coated onto the interior of a 2.6 GHz Nb cavity following the procedure developed for the flat samples. The cavity was subsequently annealed under the same conditions used for the flat samples. Cryogenic RF testing of the sputter-coated cavity demonstrated a T$_c$ of approximately 17.8 K, consistent with Nb$_3$Sn layer. Subsequently, the cavity underwent a light Sn recoating followed by a vapor diffusion Nb$_3$Sn coating process, achieving a quality factor of approximately 8.5 × 10$^9$ and an accelerating gradient of up to 11.3 MV/m at 4.2 K.

Shakel, Md Sharifuzzaman [Old Dominion U.; Jeffers↗

Top-Down Fabrication of Atomic Patterns in Twisted Bilayer Graphene

Atomic-scale engineering typically involves bottom-up approaches, leveraging parameters such as temperature, partial pressures, and chemical affinity to promote spontaneous arrangement of atoms. These parameters are applied globally, resulting in atomic-scale features scattered probabilistically throughout the material. In a top-down approach, different regions of the material are exposed to different parameters, resulting in structural changes varying on the scale of the resolution. In this work, the application of global and local parameters is combined in an aberration-corrected scanning transmission electron microscope (STEM) to demonstrate atomic-scale precision patterning of atoms in twisted bilayer graphene. The focused electron beam is used to define attachment points for foreign atoms through the controlled ejection of carbon atoms from the graphene lattice. The sample environment is staged with nearby source materials such that the sample temperature can induce migration of the source atoms across the sample surface. Under these conditions, the electron-beam (top-down) enables carbon atoms in the graphene to be replaced spontaneously by diffusing adatoms (bottom-up). Using image-based feedback control, arbitrary patterns of atoms and atom clusters are attached to the twisted bilayer graphene with limited human interaction. Finally, the role of substrate temperature on adatom and vacancy diffusion is explored by first-principles simulations.

36 MATERIALS SCIENCE↗

Polymer-assisted deposition of nanoparticle feedstocks for target fabrication

Traditional polymer-assisted deposition has been shown to produce highly uniform thin films of metal oxides, including actinide oxides. Furthermore, while producing thicker films for nuclear targets is possible through repeated coating application, we exchanged the dissolved metal species with nanoparticles to maximize the thickness that can be achieved with an individual layer. Using CeO 2 nanoparticles in a polyethyleneimine matrix, we produced targets with single-layer areal densities of 0.22 ± 0.01 mg·cm −2 (1σ) and thicknesses of 690 ± 80 nm (1σ). A custom 3D-printed spin coating chuck attachment with an inlay improved target homogeneity and will streamline future work with radioactive materials.

and nuclear chemistry↗

Effect of particle characteristics on the evolution of particle size, particle morphology, and fabric of sands loaded under uniaxial compression

This work presents the results and analyses of uniaxial compression experiments performed on three silica sands. The sands have comparable particle-size distributions, but their particles differ in morphology and strength. Cylindrical samples of the three sands were compressed in a loading device placed inside an X-ray microscope (XRM) and scanned at multiple stress levels during uniaxial compression. 3D tomography data of the samples obtained from the XRM at different stress levels were then analyzed to obtain the distributions of particle size, particle morphology, and interparticle contact normals within the sample. Results indicate that: (1) the compressibility of the sands loaded under uniaxial compression is closely tied to particle morphology and strength and (2) the anisotropy in the orientations of interparticle contact normals generally increases with axial stress; however, this increase is limited by the occurrence of particle crushing in the sample.

3D X-ray computed tomography↗

Competitive adsorption within electrode slurries and impact on cell fabrication and performance

We ask why do battery researchers use 10-20 wt% binder in research cells when commercial chemistries use much less? This report seeks to explore this question by understanding the ordering and structure of polyimide binder with a silicon/pitch-carbon black electrode system. Correlating the effect of binder concentration on electrode architecture and electrochemical properties is vital to enhancing silicon anode cycle and calendar life. Using ultra-small angle neutron scattering (USANS) and binder adsorption isotherms an optimal region of polyimide (PI) binder coverage was found. Further, there is a preferential adsorption of PI to carbon black that has to be completed before PI binds to the silicon. Optimizing the concentration of binder leads to a 50% increase in capacity due to the optimization of binder-silicon-carbon interactions.

25 ENERGY STORAGE↗

Compositionally graded aluminum-silicon alloy fabricated via friction extrusion

Herein, a novel solid-phase gradient alloying technique was developed for a high throughput composition-microstructure-mechanical property assessment. Friction extrusion of a two-piece billet setup facilitated the formation of a seamless compositionally graded aluminum (Al)-silicon (Si) extrudate rod, with Si concentration in Al matrix gradually increasing from ~1 at% at one end to ~7 at% at the other end of the rod. We observed a strong dependence of the Al grain size, morphology, and texture on the Si concentration. The Si particles pinned the recrystallized grain boundaries resulting in refined (< 10 µm) and textured grains in the high Si content region, while the Al grains in the low Si region are equiaxed, randomly textured, and with a larger average size (~50 µm). The hardness of Al-Si gradient extrudate increases by ~50% percent with a 6 at% increase in Si content due to Hall Petch and particle strengthening effects. Our approach demonstrates the use of a solid phase processing technique to successfully produce a defect-free continuously compositionally graded bulk components thus overcoming the limitations of porosity and material heterogeneities commonly observed in other techniques such as by additive laser deposition.

36 MATERIALS SCIENCE↗

Multiscale Modeling and Experimental Insights into High-Temperature Soil Biodegradation Dynamics of Semi-Crystalline Poly(Lactic Acid) Nonwoven Fabrics

This study investigates the biodegradation of semi-crystalline poly(lactic acid) (PLA) nonwovens (NWs) in soil at 58 °C using both experimental and mathematical modeling approaches. The model utilizes a system of parabolic diffusion-reaction partial differential equations (PDEs) to elucidate chemical transformations over time and in space. It accounts for phenomena such as the diffusion of water and lactic acid monomers through the polymer matrix and into the surrounding soil, along with their microbial breakdown. It also accounts for the initial PLA crystallinity and predicts its evolution in time. The model is solved numerically for a single filament, and the results were used to shed light on PLA NW transformations observed in soil over a 180-day incubation period. Various characterization techniques, including scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and Raman spectroscopy, were employed to assess morphological changes, crystallinity, and molecular changes in the NWs throughout the experiment. By comparing the experimental data with the model predictions, the hydrolysis rate coefficient was found to be 3.37 × 10 -7 s -1 , while the rate of microbial degradation of lactic acid monomers was faster, of the order of 9.63 × 10 -7 s -1 . The findings highlight the significant role of crystallinity in the biodegradation process. The PLA degradation ceases when no amorphous material remains, and the crystallinity reaches 0.8, as observed in the experiments by day 120. Furthermore, this research contributes to a deeper understanding of PLA biodegradation dynamics and offers insights for effectively managing biodegradable materials in environmental settings.

Diffusion−reaction modeling↗

Direct integration of atomic precision advanced manufacturing into middle-of-line silicon fabrication

Atomic precision advanced manufacturing (APAM) dopes silicon with enough carriers to change its electronic structure and can be used to create novel devices by defining metallic regions whose boundaries have single-atom abruptness. Incompatibility with the thermal and lithography process requirements for gated silicon transistor manufacturing have inhibited exploration of both how APAM can enhance CMOS performance and how transistor manufacturing steps can accelerate the discovery of new APAM device concepts. In this work, we introduce an APAM process that enables direct integration into the middle of a transistor manufacturing workflow. We show that a process that combines sputtering and annealing with a hardmask preserves a defining characteristic of APAM, a doping density far in excess of the solid solubility limit, while trading another, the atomic precision, for compatibility with manufacturing. The electrical characteristics of a chip combining a transistor with an APAM resistor show that the APAM module has only affected the transistor through the addition of a resistance and not by altering the transistor. This proof-of-concept demonstration also outlines the requirements and limitations of a unified APAM tool, which could be introduced into manufacturing environments, greatly expanding access to this technology and inspiring a new generation of devices with it.

Chemical vapor deposition↗

Embedded Fiber Bragg Grating (FBG) Sensors Fabricated by Ultrasonic Additive Manufacturing for High-Frequency Dynamic Strain Measurements

This article demonstrates high-frequency dynamic strain measurements using fiber Bragg grating (FBG) sensors embedded in metal parts. Using an ultrasonic additive manufacturing (UAM) process, FBGs inscribed in polyimide coated optical fibers were embedded in aluminum parts. An electromagnetic shaker was used to exert dynamic events on the embedded FBG sensors with frequencies from 1 to 10 kHz. The high-speed interrogation of FBG sensors was accomplished using a tunable vertical-cavity surface-emitting laser (VCSEL) and a high-speed interrogation system sampling at 120 kHz. The strain response measured by the FBG sensors was compared with real-time measurements using a laser velocimeter. A finite-element analysis (FEA) was performed to simulate responses to both static strain and high-frequency dynamic strain. In conclusion, results show that strains as small as 2.5$με$ can be resolved at frequencies up to 10 kHz.

36 MATERIALS SCIENCE↗

Creep-Fatigue Properties of Additional 316H PM-HIP Materials Fabricated from Different Powder Compositions and Processing Routes

The process of powder metallurgy (PM) hot isostatic pressing (HIP) works by consolidating powdered materials at relatively high temperature and pressure to form near-net-shaped components. Ideally, PM-HIP production methods can reduce component lead time and improve designs for high-temperature reactors and/or microreactors. To introduce PM-HIP into Section III, Division 5 of the American Society of Mechanical Engineers Boiler and Pressure Vessel Code, it is necessary to show adequate material properties regarding creep, high-temperature low-cycle fatigue, and creep fatigue. However, prior work has shown that the creep-fatigue cycles to failure for PM-HIP 316H stainless steel are greatly reduced compared to the conventional, wrought product. This work continued creep-fatigue analysis on a 316H stainless steel with lower oxygen and nitrogen contents and at different HIP parameters than previously analyzed. The objective was to better understand what is causing the reduced PM-HIP 316H performance so improvements can be made PM-HIP 316H creep-fatigue lifetimes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗