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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 451 records · Page 25

Additive Manufacturing of Lattice Structures for Catalyst Applications

Abstract The design and fabrication of Inconel 718 open-pore lattice structures via Laser Powder Bed Fusion (LPBF) has been investigated in this research, focusing on applications such as catalyst supports in jet fuel production. The study explores the impact of laser power and scanning speed on the geometrical resolution of these structures aiming to achieve high porosity (porosity > 60%) and specific pore sizes ranging from 500–1000 μm, intending to serve as catalyst supports, replacing conventionally manufactured foams to reduce costs. Results demonstrate the significant influence of processing parameters on the geometrical aspects of printed lattice structures, with laser power having a more pronounced effect on geometrical accuracy than scanning speed. Additionally, the mechanical properties of the printed lattice structures showed a correlation with the lattice strut sizes, as lattices with less porosity and thicker struts resulted in higher maximum shear stress.

36 MATERIALS SCIENCE↗

Electron-hole asymmetry in the phase diagram of carrier-tuned CsV3Sb5

In this work, we study the effect of electron doping on the kagome superconductor CsV 3 Sb 5 . Single crystals and powders of CsV 3 Sb 5− x Te x are synthesized and characterized via magnetic susceptibility, nuclear quadrupole resonance, and x-ray diffraction measurements, where we observe a slight suppression of the charge density wave transition temperature and superconducting temperature with the introduction of electron dopants. In contrast to hole doping, both transitions survive relatively unperturbed up to the solubility limit of Te within the lattice. A comparison is presented between the electronic phase diagrams of electron- and hole-tuned CsV 3 Sb 5 .

36 MATERIALS SCIENCE↗

Mechanical Activation and Cation Site Disorder in MgAl 2 O 4

The synthesis and crystallographic site occupancy were investigated for MgAl 2 O 4 with and without mechanical activation of the precursor powders. Heating to 1200 °C or higher resulted in the formation of a single spinel phase regardless of whether the powders were mechanically activated or not. Neutron diffraction analysis was used to determine cation site occupancy and revealed that mechanical activation resulted in a lower degree of cation site inversion compared to the nonactivated materials, which indicated that the powders were closer to thermodynamic equilibrium. This is the first study to characterize the effects of mechanical activation on crystallographic site occupancy in magnesium aluminate spinel using neutron diffraction.

36 MATERIALS SCIENCE↗

Characterization of Additively Manufactured Tungsten Heavy Alloy Material (CRADA Final Report)

LLNL and Aerojet Rocketdyne, Inc. (AR), using earlier collaborative work in powder bed printing of other materials, have been collaboratively pursuing the additive manufacture of tungsten heavy alloy (WHA) material since 2014. The goal of the project was to establish the ability to produce the LLNL developed material at the AR production facility. When accomplished, AR would produce an agreed array of test samples to technically characterize the material properties via testing. AR would conduct a portion of that testing and provide those results to LLNL. The goal of this work was to perform a trial transfer of LLNL’s WHA technology to AR

36 MATERIALS SCIENCE↗

Characterization of Large Batch 14YWT Heat (NFA-2) for JOYO Irradiations (Rev.1)

The development and deployment of advanced cladding materials in advanced reactors requires the collection of relevant performance data for each cladding concept. Novel cladding concepts typically undergo significant innovation and iteration over the course of their development, and intention should be given to providing a snapshot of present performance. Thus, a modern heat of the nanostructured ferritic alloy (NFA) 14YWT is produced using state-of-the-art procedures for impurity minimization combined with thermomechanical processing methods designed to optimize fracture toughness, tensile strength, and ductility. This new heat of 14YWT, NFA-2, will provide the Advanced Fuels Campaign with adequate material for upcoming irradiation and mechanical testing campaigns. This report outlines procurement of new gas atomized 14YWT powder, production of four new bars of 14YWT, and subsequent mechanical and microstructural property characterization.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Structure determination of two structural analogs, named 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16F2N4S) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4-b]-1,3,4-thiadiazole (C23H16ClFN4S) by synchrotron X-ray powder diffraction

Two novel compounds, 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-fluorophenyl)-1,2,4-triazolo[3,4- b ]-1,3,4-thiadiazole (C 23 H 16 F 2 N 4 S) ( 1 ) and 3-[1-(2-fluoro-4-biphenyl)ethyl]-6-(4-chlorophenyl)-1,2,4-triazolo[3,4- b ]-1,3,4-thiadiazole (C 23 H 16 ClFN 4 S) ( 2 ), have been designed and synthesized as cytotoxic agents. The compounds were characterized by infrared, proton nuclear magnetic resonance, mass spectral data, elemental analysis and X-ray powder diffraction. The present study comprises spectral data and crystal structures of these novel compounds determined from synchrotron X-ray powder diffraction data. The structure solutions were obtained by simulated annealing. The final structures were achieved by Rietveld refinement using soft restraints for all bond lengths, bond angles, and planar groups. Both compounds crystallize in space group $P\bar 1$ , Z = 2, with the unit-cell parameters a = 6.37433(9), b = 11.3641(2), c = 14.09115(19) Å, α = 80.1740(8)°, β = 85.1164(8)°, γ = 80.9831(10)°, V = 991.55(3) Å 3 of compound ( 1 ) and a = 6.53736(6), b = 11.55725(15), c = 14.01373(13) Å, α = 80.3323(7)°, β = 84.8939(6)°, γ = 79.3954(8)°, V = 1024.08(2) Å 3 of compound ( 2 ). Structural analyses reveal that the title compounds are isostructural.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Identifying point defects and ordering in the high-entropy layered oxide Li 1.5 MO 3-δ (M=Mn, Al, Fe, Co, Ni) for energy storage applications

High-entropy layered oxides (HELOs) represent a very promising class of next-generation battery cathodes, combining the well-studied properties of layered cathode materials such as LiCoO 2 with the chemical tunability and stability of high-entropy materials. HELO materials often form particles with complex defects and domain structures, complicating accurate characterization of structure and cation mixing. Understanding disorder and order in HELO materials is necessary for understanding their performance and utility as cathodes. Here we demonstrate the characterization of the HELO Li 1.5 MO 3-δ (M = Mn, Al, Fe, Co, Ni), wherein X-ray powder diffraction, transmission electron microscopy imaging, and electron diffraction patterns are analyzed to reveal the presence of ordering in the HELO, with imaging and diffraction simulation employed to compare experimental results to atomic modeling. Finally, without rigorous characterization at the atomic scale, important features such as defect ordering can be easily overlooked and therefore remain unconsidered when interpreting experimental results.

36 MATERIALS SCIENCE↗

Morphology evolution of γ′ precipitates in a powder metallurgy Ni-base superalloy

Highlights: • The 3-D morphology of the γ′ precipitate for the Ni-base superalloy was characterized using the electronic etching. • Various morphologies of the γ′ precipitates, including cuboids, octet and dendritic shape, were observed. • Cooling rate has a significant influence on the morphology of the γ′ precipitate. • When the cooling rate was lower than 6 °C/min, the dendritic shape γ′ with eight-primary-branch pattern was observed. - Abstract: Effect of the cooling rate on the morphological evolution of the γ′ precipitate in a powder metallurgy Ni-base superalloy FGH96 was studied. Results showed that as the cooling rate decreased from 600 °C/min to 2 °C/min, the precipitate morphology transformed from sphere to cuboid, octet and dendrite. As the cooling rate increased, the mean size of the γ′ precipitates decreased while the nucleation density increased. When the cooling rate was lower than 6 °C/min, the precipitate would evolve from a sphere to cuboids with concave faces, octets, dendrite to final split-off branches. The morphological transition was driven by energy balance between coherent strain induced by the γ′/γ lattice misfit and interface energy. The dendritic shape γ′ exhibited an eight-primary-branch pattern with preferred growth direction along <111>, and secondary arms along <100>.

36 MATERIALS SCIENCE↗

Superconducting Performance, Structure, Microstructure, and Trapped Field of Top-Seeded Melt-Processed Bulk Y{sub 3}Ba{sub 5}Cu{sub 8}O{sub x}

The sintering temperature for the production of Y{sub 3}Ba{sub 5}Cu{sub 8}O{sub 18} (Y-358) preform powders synthesized in sol-gel spontaneous combustion technique was optimized. A large single-grain bulk Y-358 crystal was fabricated employing a top-seeded melt-growth technique utilizing the optimally sintered preform powders (i.e., at 900 {sup ∘}C for 12 h). Structural, microstructural, elemental, and magnetic properties were investigated by means of X-ray diffraction, scanning electron microscopy, and SQUID, respectively. The structural characterization indicated that the sample is highly textured in (00l) direction. The Y-358 phase fractions were estimated in both preform powders and bulk sample using Rietveld refinement. The onset of superconducting transition is observed at 92.5 K, and the curve is very sharp indicative of the high quality of the produced bulk sample. The field dependence of critical current density (J{sub c}) was determined at 77 K, and the self-field J{sub c} was found to be ∼26 kA/cm{sup 2}. A magnetic field of 0.27 T was trapped by the sample at 77 K.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Enhanced Photocatalytic Degradation of Methylene Blue Dye, Opto-magnetic and Antibacterial Behaviour of Pure and La-doped ZnO Nanoparticles

The different doping concentrations of lanthanum (La)-doped ZnO nanoparticles were synthesized successfully using zinc acetate and lanthanum nitrate via wet chemical method. Characterization of the prepared sample was done by standard analytical techniques such as powder x-ray diffraction analysis (P-XRD), high-resolution scanning electron microscopy (HR-SEM), energy-dispersive spectroscopy (EDS), Fourier transformer-infrared (FT-IR) spectroscopy, photoluminescence (PL) and UV-Vis spectroscopy (UV-Vis), and magnetic studies (VSM). The structural analysis has been carried out by powder x-ray diffraction. X-ray diffraction studies revealed that the nanoparticles are well-crystalline and possess hexagonal wurtzite structure. HR-SEM images showed the homogenous spherical-shaped morphology of the synthesized ZnO nanoparticles. EDS analysis confirmed the presence of La ions into ZnO lattice. The band gap (Eg) energy was determined by UV-Visible spectral data, and it was found that the Eg value decreases with increasing the La concentration into ZnO lattice. PL spectra confirmed that the effective La doping enhance the UV and visible region near band gap emission. The effect of La doping on the photocatalytic activity of ZnO nanoparticles for the degradation of methylene blue dye was studied under solar illumination and the results showed that the La doping kindles appreciable degradation of MB. The optical density measurements of the ZnO nanoparticles against both gram-positive (Bacillus subtilis, Staphylococcus aureus) as well as gram-negative bacteria (Proteus mirabilis, Salmonella typhi) showed better bacterial activity than pure ZnO. Moreover, it showed that higher dopant La in ZnO exhibit efficient antibacterial activity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Migration of Al within dealuminated beta extruded catalysts influences olefin distribution during ethanol upgrading

Zeolites serve as essential catalytic platforms for many industrial processes, including emerging ethanol-to-olefins (ETO) upgrading technologies. Although metal-loaded (Cu, Zn, Y) dealuminated beta (deAlBeta) zeolite powders are promising catalysts for direct ETO conversion with high selectivity to butene-rich C3+ olefins necessary for production of sustainable aviation fuels (SAF), development of these materials as shaped technical bodies through the incorporation of binders is required for scale-up and commercial viability. Here, we report the ethanol upgrading performance of Cu-Zn-Y/deAlBeta extruded catalysts formulated with either alumina or kaolin clay binders. Both extrudates exhibit high ethanol dehydration reactivity which competes with the initial ethanol dehydrogenation step in the direct ETO reaction network. Consequently, elevated selectivity to dehydration side products (ethylene, diethyl ether) at ∼100% ethanol conversion is observed on Cu-Zn-Y/deAlBeta extrudates compared to the powder catalyst, which inhibits production of desired C3+ olefins. Utilizing microscopy and spectroscopic characterizations, we attribute this to Al migration from binder to zeolite particles within the extrudates, thus re-aluminating the zeolite and generating Brønsted acid sites active for dehydration reactions. This work elucidates the effects of binder incorporation on ETO product distributions and emphasizes that binder selection must be carefully considered during design of extruded zeolite catalysts.

Jacobs, Hunter [ORNL] (ORCID:000000016190874X)↗

Conversion of (NH 4 ) 2 [ReF 6 ] into ReO 2 mixed phases: A thermal analysis study

We report the thermal behavior of (NH 4 ) 2 [ReF 6 ] was evaluated in an alumina crucible using simultaneous thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC) in an argon atmosphere. The TGA of (NH 4 ) 2 [ReF 6 ] is characterized by a single step decomposition while the DSC exhibits two exothermic peaks. Powder X-ray diffraction (PXRD) analyses of the decomposition products show the presence of a mixed ReO 2 phase. The formation of ReO2 is driven by the reaction of (NH 4 ) 2 [ReF 6 ] with Al 2 O 3 at the grain boundary of the alumina crucible. XRD peak broadenings due to the combined effect of crystallite size and lattice strain were evaluated using both Scherrer and Williamson-Hall methods.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Understanding the effect of salt concentrations on fast charging performance of Li-ion cells

Here, different lithium salt (lithium bis(fluorosulfonyl) imide (LiFSI)/LiPF 6 9/1 mol ratio) concentrations in carbonate electrolyte were studied on the fast charging performance of LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622)/graphite pouch cells. The cells with electrolyte concentration from 0.75 M to 1.50 M showed similar fast charging capabilities. Further increase of the concentration to 1.75 M and 2.00 M decreased the attainable capacity in fast charging. In the long-term cycling test, the capacity retention after 200 fast charging cycles increased with the increase of salt concentration in electrolyte. Cells with 1.5 M electrolyte showed the best overall performance in fast charging capacity and long-term cycling. Li platings were observed in the cells with 0.75 M, 1.00 M and 1.25 M electrolyte. It was improved with greatly reduced Li plating area in 1.50 M, and no Li plating at all in 1.75 M and 2.00 M electrolyte. Post-mortem analysis such as neutron powder diffraction (NPD) and X-ray photoelectron spectroscopy (XPS) were used to characterize the electrode after cycling. It suggests that electrolyte concentration needs to be optimized for a given cell configuration with specific electrode and loading.

25 ENERGY STORAGE↗

Syntheses, structures and selective dye adsorption of five formic-based coordination polymers prepared by in-situ hydrolysis of N, N′-dimethylformamide

Five functional coordination polymers (formic-based CPs) namely: ([Cu{sub 2}(CHOO){sub 3}(bibp){sub 2}]·CHOO){sub n} (1), ([Co{sub 2}(CHOO){sub 3}(bibp){sub 2}]·NO{sub 3}·H{sub 2}O)n (2), ([Ni{sub 2}(CHOO){sub 3}(bibp){sub 2}]·NO{sub 3}·H{sub 2}O){sub n} (3) [Co(CHOO){sub 2}(bbibp)]{sub n} (4) and [Zn(CHOO){sub 2}(bbibp)]{sub n} (5) (bibp=4,4′-bis(imidazolyl)biphenyl, bbibp=4,4′-bis(benzoimidazo-1-yl)biphenyl) have been successfully hydrothermally synthesized using the in-situ hydrolysis of N, N′-dimethylformamide (DMF) as the source of formate. All of these five polymers were characterized by single-crystal X-ray diffraction, elemental analysis, IR spectra, powder X-ray diffraction (PXRD), and thermogravimetric (TG) analysis. Complexes 1–3 have the similar three-dimensional 3D kag topological framework built from the bibp ligand as the support member between the neighboring formic planes. Both complexes 4 and 5 have the similar one-dimensional 1D linear chain which is further assembled into 3D supermolecular structure by C–H…O hydrogen bonds. The dyes adsorption experiments have also been investigated systematically. The results show that complexes 2 and 3 exhibit high selective adsorption ability towards anionic dyes in their aqueous solution. Moreover, complex 2 displays good reversibility in the process of the dyes adsorption-release. Meanwhile, the unusual blocking phenomenon was firstly observed when complex 2 was in MO/OIV aqueous solutions with different concentration.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

In situ growth of ceramic quantum dots in polyaniline host via water vapor flow diffusion as potential electrode materials for energy applications

In situ preparation of polyaniline-ceramic nanocomposites has recently demonstrated that the electrical properties are highly improved with respect to the typical ex situ preparations. In this report, we present for the first time, to the best of our knowledge, the in situ growth of titanium oxide quantum dots in polyaniline host via water vapor flow diffusion as an easily adaptable route to prepare other ceramic-polymer nanocomposites. The main relevance of this method is the possibility to prepare ceramic quantum dots from alkoxide precursors using water vapor flow into any hydrophobic polymer host and to achieve good homogeneity and size-control. In addition, we perform full characterization by means of high-resolution transmission electron microscopy, X-ray powder diffraction, small angle X-ray scattering, thermogravimetric and calorimetric analyses, confocal Raman microscopy and impedance spectroscopy analyses. The presence of the polymer host and interparticle Coulomb repulsive interactions was evaluated as an influence for the formation of ~3–8 nm equally-sized quantum dots independently of the concentration. The polyaniline polaron population showed an increase for the quantum dots diluted regime and the suppression at the concentrated regime, ascribed to the formation of chemical bonds at the interface, which was confirmed by theoretical simulations. In agreement with the previous observation, the in situ growth of ceramic quantum dots in polyaniline host via water vapor flow diffusion could be very useful as a novel approach to prepare electrode materials for energy conversion and storage applications. - Highlights: • In situ growth of titanium oxide quantum dots in polyaniline host via water vapor flow diffusion. • Polyaniline charge carriers at the interface and charge interactions between quantum dots. • Easy extrapolation to sol-gel derived quantum dots into polymer host as potential electrode materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Moisture on Dopant Segregation in Solid Hosts

Transition metal-doped semiconductor materials are extensively employed for light harvesting and photocatalytic applications owing to their increased light absorption and charge mobility. Here, spatial tailoring of the Ni dopant in TiO 2 nanostructures is performed by varying the secondary processing parameters to engineer the resulting optoelectronic properties for select applications. Specifically, the aging of the dried Ti sol and the resulting Ni segregation are observed to be moisture-driven phenomena based on the infrared and time-resolved UV–vis spectroscopy measurements. While X-ray diffraction and scanning transmission electron microscopy coupled with electron energy-loss spectroscopy characterizations show a clear difference in the crystal structures between pristine TiO 2 powders and phase-segregated NiO–TiO 2 , the thermogravimetric measurements reveal substitution of the ethoxy group by ambient moisture, resulting in the ejection of hydroxylated Ni clusters. Moreover, the doped system could be locked into a metastable state by rapidly annealing the amorphous powders. Lastly, the photocatalytic activity of these different TiO 2 :Ni 2+ (15 mol %) nanoparticles under AM 1.5G solar light highlights the relationship between the photocatalytic activity and the dopant position. This ability to spatially control dopants within highly doped materials allows for direct control of specific optoelectronic properties, paramount for photoelectrochemical devices.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Effect of Gd substitution on the structural, magnetic, and magnetocaloric properties of HoCrO 3

Rare-earth chromites are a novel type of magnetoelectric multiferroics. Here, a Ho 0.33 Gd 0.67 CrO 3 powder sample was synthesized via a citrate route, and the structural properties were characterized by X-ray diffraction, scanning electron microscopy, and the Raman technique. The UV-Visible optical absorbance spectra were also measured in the wavelength range of 200–800 nm. The valence state of Cr was found to be purely 3+ according to the X-ray photoelectron spectroscopy. The temperature-dependent dielectric constant and loss tangent data measured between the frequencies of 1 kHz and 1 MHz show no anomalies around the magnetic transition temperature of the material. The dc magnetization measurements show that the ordering temperature of Cr 3+ ( T N C r ) is 155 K for Ho 0.33 Gd 0.67 CrO 3 , which is larger than 140 K for HoCrO 3 . The positive slope of the Arrott plots from 0 T to 7 T reveals that the antiferromagnetic-paramagnetic phase transition is second-order in nature. At a field of 7 T, the Ho 0.33 Gd 0.67 CrO 3 sample showed a giant magnetocaloric entropy change, -ΔS, of ~23.3 J/kg K at 5 K, and a refrigeration capacity of ~481.2 J/kg, which are much higher than those of pure bulk HoCrO 3 . This renders this material prospective for magnetic refrigeration in the low temperature (<30 K) range.

36 MATERIALS SCIENCE↗