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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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226 records · Page 13
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Capability to Process and Characterize Uranium-Zirconium (U-Zr) and Uranium-Zirconium-Plutonium (U-Zr-Pu) Alloys

This work investigated co-reduction of anhydrous compounds of uranium, zirconium, and plutonium to produce uranium rich ternary nuclear fuel alloys. Metallothermic co-reduction is a novel method to produce all-metal nuclear fuels. Metal fuels offer thermal, fissility, compatibility, and security benefits over oxide fuels. Alloys of uranium–10% zirconium with plutonium contents of 0%, 2.5%, 5%, and 10% were produced, with yields of 60–85% of theoretical values in a traditional calciothermic bomb reduction apparatus. Microstructural analysis indicated transformation of uranium phase from gamma to beta and then alpha, in alternating lamellar plates typical of alpha phase uranium and delta phase uranium-zirconium, with zirconium and carbides at prior grain boundaries. Some of the analyses were inconclusive in their results and therefore require additional testing. Successful ternary co-reduction would simplify production of homogeneous feedstock and thereby streamline manufacture of homogeneous ternary metallic fuel.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2024

Fundamentals of Scalable Nanoparticle Assembly in Engineering Polymres

Systematically improving the properties of polymer nanocomposites is contingent on effectively controlling nanoparticle (NP) dispersion; further, it is necessary to attain this at scale if these methods are to impact practical applications. While most past work has focused on amorphous polymers, ≈ 70% of all polymers sold annually are semicrystalline. Inspired by this apparent disconnect, our work in the current DOE funded grant and this renewal proposal employs a novel handle, polymer crystallization, to organize NPs into the various amorphous zones of the lamellar semicrystalline morphology (interlamellar, interfibrillar and interspherulitic domains) of stereoregular polymers. We hypothesize that the isothermal crystallization rate of a polymer host, G, and NP diffusivity, are the two relevant control parameters in this context. In the case where the NPs are miscible in the melt, they remain spatially well-dispersed when the polymer is crystallized at a rate that is fast relative to NP diffusion. In contrast, monolayer-thick NP sheets with intersheet spacing of ~10-100nm form in slowly crystallized samples. This sheet stacking is remarkably similar to that seen in natural materials, e.g., Nacre. There is also ordering of the NPs at the larger interfibrillar scale. Importantly, the relative fraction of engulfed, interlamellar and interfibrillar NPs is determined by G. Further, the modulus of these materials can increase by a factor of 2-3 due to the organization state of the NPs, while leaving fracture toughness unaffected. We have established the broad applicability of this approach in two polymers, polyethylene (PE) and polyethyleneoxide (PEO). To achieve this goal we developed a method for grafting long PE chains from NPs with controlled graft density and molecular weight, giving us the ability to tailor their dispersion in the PE melt prior to crystallization. In this renewal proposal, we will develop the fundamental, quantitative understanding that will allow us to independently tailor polymer crystallization rate, NP diffusivity and NP agglomeration state in semicrystalline polymers so as to facilely control NP ordering and hence properties. A program that tightly integrates experiment and theory is proposed, and a key outcome of this research will be a three-dimensional design map for different regimes of NP organization (and hence properties) that can be achieved by polymer crystallization. A second independent outcome is the role of directional solidification and how it competes with the rates of polymer crystallization and NP mobility to affect the organization of the NP.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Self-assembled nanofiltration membranes with thermo- and pH-responsive behavior

We produce controlled nanostructured membranes from cross-linking of self-assembled diacrylated poloxamers. At sufficiently high concentrations, poloxamers form lyotropic liquid crystals (LLCs), such as lamellar (L α ), cubic packing of spherical micelles, and hexagonal packing of rod-like micelles in water (H 1 ). We use the H 1 phase as a template to produce orderly packed nanofibrous membranes. The obtained membrane has a continuous 3D transport pathway and can alter its nanofiltration (NF) properties in response to changes in temperature and pH. The formulation includes Pluronic P84-diacrylate (P84DA), a thermoresponsive component that acts as both macromer and structure-directing amphiphile. P84DA facilitates changes in membrane pore size with temperature due to its thermoresponsiveness when it is in contact with water. Furthermore, the precursor contains acrylic acid (AAc) as the charged component, which upon copolymerization with P84DA, not only enables ion separation through Donnan exclusion but also imparts pH-responsive behavior for the separation of ionic species. The membrane performance is studied and compared with a commercial NF membrane (NF270). We show that the synthesized NF membrane has separation properties adjustable with temperature and pH with exceptional resistance to fouling by various solutes due to its highly hydrophilic surface. Furthermore, the membrane shows an outstanding sulfate over chloride ion selectivity, which is a requirement for salt fractionation applications. Deducted from separate experiments, the ideal chloride/sulfate selectivity for magnesium cation is about 2.38 at low ionic strengths. This study is done on a model system to show the capability of incorporating pH-responsiveness in LLC templated membranes, in which the pH-responsive range can be designed by changing the charged groups of comonomer in the formulation.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Rapid Fabrication of High Frame Rate Multichannel FTIR Spectrometers

Spectrally resolved signals in the short- to mid-wave infrared (SWIR/MWIR) bands at high-temporal resolution are critical for many national security remote sensing missions. Currently available off the shelf technology can achieve either high temporal resolution or high spectral resolution, but rugged instruments that can achieve both simultaneously remain mostly in the realm of one-off R&D projects. This report documents efforts to demonstrate a new technique for designing and building high resolution, high framerate multichannel FTIR (MC-FTIR) spectrometers that operate in the SWIR/MWIR bands. The core optical element in a MC-FTIR spectrometer is an array of statically-tuned lamellar grating interferometers (LGI). In the original MC-FTIR work these arrays were fabricated using a synchrotron x-ray lithography method. We proposed to instead fabricate these LGI arrays using multiphoton lithography (MPL), a 3D printing technique that can fabricate meso-scale structures with sub-micron precision. Although we were able to fabricate LGI arrays of sufficient size using MPL, the realized optical surfaces had unsuitably high optical form errors, precluding their use in a fieldable instrument. Further advancement in MPL technology may eventually enable fabrication of interferometer-grade LGI arrays.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2020

Chemical and Structural Changes in Corn Stover After Ensiling: Influence on Bioconversion

Production of biofuels, bioproducts, and bioenergy requires a well-characterized, stable, and reasonably uniform biomass supply and well-established supply chains for shipping biomass from farm fields to biorefineries, while achieving year-round production targets. Preserving and stabilizing biomass feedstock during storage is a necessity for cost-effective and sustainable biofuel production. Ensiling is a common storage method used to preserve and even improve forage quality; however, the impact of ensiling on biomass physical and chemical properties that influence bioconversion processes has been variable. Our objective in this work was to determine the effects of ensiling on lignocellulosic feedstock physicochemical properties and how that influences bioconversion requirements. We observed statistically significant decreases (p < 0.05) in the content of two major structural carbohydrates (glucan and xylan) of 5 and 8%, respectively, between the ensiled and non-ensiled materials. We were unable to detect differences in sugar yields from structural carbohydrates after pretreatment and enzymatic hydrolysis of the ensiled materials compared to non-ensiled controls. Based on this work, we conclude that ensiling the corn stover did not change the bioconversion requirements compared to the control samples and incurred losses of structural carbohydrates. At the light microscopy level, ensiled corn stover exhibited little structural change or relocation of cell wall components as detected by immunocytochemistry. However, more subtle structural changes were revealed by electron microscopy, as ensiled cell walls exhibit ultrastructural characteristics such as wall delimitation intermediate between non-ensiled and dilute-acid-pretreated cell walls. These findings suggest that alternative methods of conversion, such as deacetylation and mechanical refining, could take advantage of lamellar defects and may be more effective than dilute acid or hot water pretreatment for biomass conversion of ensiled materials.

09 BIOMASS FUELS↗
DOE OSTI2021

Mechanical Behavior Assessment of Ti-6Al-4V ELI Alloy Produced by Laser Powder Bed Fusion

The present work correlates the quasi-static, tensile mechanical properties of additively manufactured Ti-6Al-4V extra low interstitial (ELI, Grade 23) alloy to the phase constituents, microstructure, and fracture surface characteristics that changed with post-heat treatment of stress relief (670 °C for 5 h) and hot isostatic pressing (HIP with 100 MPa at 920 °C for 2 h under an Ar atmosphere). Ti-6Al-4V ELI alloy tensile specimens in both the horizontal (i.e., X and Y) and vertical (Z) directions were produced by the laser powder bed fusion (LPBF) technique. Higher yield strength (1141 MPa), higher tensile strength (1190 MPa), but lower elongation at fracture (6.9%), along with mechanical anisotropy were observed for as-stress-relieved (ASR) samples. However, after HIP, consistent and isotropic mechanical behaviors were observed with a slight reduction in yield strength (928 MPa) and tensile strength (1003 MPa), but with a significant improvement in elongation at fracture (16.1%). Phase constituents of acicular α' phase in ASR and lamellar α + β phases in HIP samples were observed and quantified to corroborate the reduction in strength and increase in ductility. The anisotropic variation in elongation at fracture observed for the ASR samples, particularly built in the build (Z) direction, was related to the presence of “keyhole” porosity.

42 ENGINEERING↗
DOE OSTI2020

Hybrid Unilamellar Vesicles of Phospholipids and Block Copolymers with Crystalline Domains

Phospholipid (PL) membranes are ubiquitous in nature and their phase behavior has been extensively studied. Lipids assemble in a variety of structures and external stimuli can activate a quick switch between them. Amphiphilic block copolymers (BCPs) can self-organize in analogous structures but are mechanically more robust and transformations are considerably slower. The combination of PL dynamical behavior with BCP chemical richness could lead to new materials for applications in bioinspired separation membranes and drug delivery. It is timely to underpin the phase behavior of these hybrid systems and a few recent studies have revealed that PL–BCP membranes display synergistic structural, phase-separation, and dynamical properties not seen in pure components. One example is phase-separation in the membrane plane, which seems to be strongly affected by the ability of the PL to form lamellar phases with ordered alkyl chains. In this paper we focus on a rather less explored design handle which is the crystalline properties of the BCP component. Using a combination of confocal laser scanning microscopy and X-ray scattering we show that hybrid membranes of 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) and methoxy-poly(ethylene glycol)-b-poly(ε-caprolactone) (mPEG-b-PCL) display BCP-rich and PL-rich domains when the BCP comprises crystalline moieties. The packing of the hydrophilic part of the BCP (PEG) favors mixing of DPPC at the molecular level or into nanoscale domains while semi-crystalline and hydrophobic PCL moieties bolster microscopic domain formation in the hybrid membrane plane

phase-separation↗
DOE OSTI2021

Structure and Interdigitation of Chain-Asymmetric Phosphatidylcholines and Milk Sphingomyelin in the Fluid Phase

We addressed the frequent occurrence of mixed-chain lipids in biological membranes and their impact on membrane structure by studying several chain-asymmetric phosphatidylcholines and the highly asymmetric milk sphingomyelin. Specifically, we report trans-membrane structures of the corresponding fluid lamellar phases using small-angle X-ray and neutron scattering, which were jointly analyzed in terms of a membrane composition-specific model, including a headgroup hydration shell. Focusing on terminal methyl groups at the bilayer center, we found a linear relation between hydrocarbon chain length mismatch and the methyl-overlap for phosphatidylcholines, and a non-negligible impact of the glycerol backbone-tilting, letting the sn1-chain penetrate deeper into the opposing leaflet by half a CH 2 group. That is, penetration-depth differences due to the ester-linked hydrocarbons at the glycerol backbone, previously reported for gel phase structures, also extend to the more relevant physiological fluid phase, but are significantly reduced. Moreover, milk sphingomyelin was found to follow the same linear relationship suggesting a similar tilt of the sphingosine backbone. Complementarily performed molecular dynamics simulations revealed that there is always a part of the lipid tails bending back, even if there is a high interdigitation with the opposing chains. The extent of this back-bending was similar to that in chain symmetric bilayers. For both cases of adaptation to chain length mismatch, chain-asymmetry has a large impact on hydrocarbon chain ordering, inducing disorder in the longer of the two hydrocarbons.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Solvothermal synthesis of metal alkanoate and metal oxide nanoparticles

A facile solvothermal method can be used to synthesize metal alkanoate nanoparticles using a metal nitrate precursor, alcohol/water, and alkanoic acid. The method can produce lanthanide (e.g., La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, or Yb) and transition metal (e.g., Ag, Co, Cu, or Pb) alkanoate nanoparticles (<100 nm) with spherical morphology. These hybrid nanomaterials adopt a lamellar structure consisting of inorganic metal cation layers separated by an alkanoate anion bilayer and exhibit liquid crystalline phases during melting. The metal alkanoate nanoparticles can be calcined to produce metal oxide nanoparticles.

Treadwell, LaRico Juan↗
DOE OSTI2024

High-resolution chemical patterns from negative tone resists for the integration of extreme ultraviolet patterns of metal-oxide resists with directed self-assembly of block copolymers

Extreme ultraviolet (EUV) lithography faces significant challenges in designing suitable resist materials that can provide adequate precision, while maintaining economically viable throughput. These challenges in resist materials have led to printing failures and high roughness in EUV patterns, compromising the performance of semiconductor devices. Integrating directed self-assembly (DSA) of block copolymers (BCPs) with EUV lithography offers a promising solution because, while the BCPs register to the EUV-defined chemical guiding pattern, the thermodynamically determined structures of the BCPs automatically rectify defects and roughness in the EUV pattern. Despite the superior resolution of metal-oxide EUV resists (MORs), their application to DSA is limited by the difficulty in converting them into chemical patterns that allow effective transfer of the rectified patterns of DSA films into inorganic materials. To address this challenge, this study introduces a novel strategy for fabricating chemical patterns using hydrogen silsesquioxane (HSQ), a high-resolution negative tone inorganic resist, as a model system for MORs. Initially, a sacrificial Cr pattern is generated from HSQ patterns via reactive ion etching. The sacrificial Cr pattern is converted into a chemical pattern by first grafting a water-soluble polyethylene oxide brush onto the substrate, then wet etching the Cr, and finally grafting nonpolar polystyrene brushes. Assembling polystyrene-block-poly(methyl methacrylate) on these patterns results in structures oriented and registered with the underlying pattern, achieving 24 nm full-pitch resolutions. In conclusion, this approach has the potential to integrate MOR patterns into the DSA process, thereby enabling the generation of high-quality sub-10 nm patterns with high-χ BCPs.

Atomic force microscopy↗