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At least 1,369 records · Page 76
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Contributions to the mechanistic understanding of the microstructural evolution in irradiated U-Mo dispersion fuel

Here, advanced microstructural characterization techniques, such as scanning electron microscopy (SEM) and scanning transmission electron microscopy - energy dispersive x-ray spectroscopy (STEM-EDS), were used to interpret the fuel microstructure evolution and fission products behavior in U-Mo dispersion fuel irradiated in the Advanced Test Reactor (ATR) as part of the European Mini-Plate Irradiation Experiment (EMPIrE) test. The larger as-fabricated fuel grain size achieved by heat-treating the U-Mo powder resulted in slower high burnup structure (HBS) development and reduced fission gas porosity. Slower HBS kinetics was observed at the fuel kernels’ periphery, which contained smaller and less fission gas bubbles at all fission densities (FDs) investigated and was attributed to a locally reduced damage density and fission products concentration, as corroborated with Monte Carlo simulations. The non-refined grains at the fuel kernel periphery hosted a perfectly ordered fission Gas Bubble Superlattice (GBS) up to 6.3 × 10 21 fissions/cm 3 . Nano-scale STEM-EDS analysis presented in this study provided useful information on the GBS characteristic morphology and evolution in U-Mo fuel. The concentration of fission gas in the GBS progressively increased with FD, pointing to an evolution of the nanobubble pressure status with irradiation. A possible connection between the GBS collapse and HBS onset is proposed for which there exists a threshold in the misorientation of the refined sub-grains above which the GBS stability during irradiation is no longer preserved, resulting in the GBS collapse.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Understanding the Hydronium Cation in the Solid State: A Study in Synthetic Hydronium Uranyl Phosphate and Arsenate Mineral Systems and Their Irradiation Stability

Here, we present neutron diffraction, electronic structure calculations, and optical vibrational spectroscopic characterization of hydronium uranyl phosphate (HUP), the synthetic analog of chernikovite ((H 3 O)(UO 2 )(PO 4 )·3H 2 O) to gain insight into structural features of the hydronium cation in the solid state. HUP crystallizes in P2 1 /c instead of previously reported P4/ncc 1 at room temperature and Pccn below 302 K. Lower symmetry was required due to hydronium and interstitial water positions within the structure. Crystallographic positions of hydronium cations determined from powder neutron diffraction data are bolstered by Raman and attenuated total reflectance infrared spectroscopic measurements and are further informed by density functional theory with phonon eigenvector analysis for spectral assignments. Finally, HUP and its arsenate analog (trogerite, (H 3 O)(UO 2 )(AsO 4 )·3H 2 O), (HUAs) were studied using He 2+ irradiation as an analog for α radiolysis to investigate the irradiation stability of these phases and the stability of hydronium cations in the solid state. Dose studies were employed wherein each sample was irradiated to 5, 10, 15, 25, and 50 MGy. Structural insight regarding irradiated materials is gained using optical vibrational spectroscopy and powder X-ray diffraction. Surprising irradiation stability of HUAs was found up to 50 MGy of dose, which may have important implications for understanding and modeling the geologic stability of legacy U.

actinides↗
DOE OSTI2016

Natural abundance 14 N and 15 N solid-state NMR of pharmaceuticals and their polymorphs

14 N ultra-wideline (UW), 1 H{ 15 N} indirectly-detected HETCOR (idHETCOR) and 15 N dynamic nuclear polarization (DNP) solid-state NMR (SSNMR) experiments, in combination with plane-wave density functional theory (DFT) calculations of 14 N EFG tensors, were utilized to characterize a series of nitrogen-containing active pharmaceutical ingredients (APIs), including HCl salts of scopolamine, alprenolol, isoprenaline, acebutolol, dibucaine, nicardipine, and ranitidine. Here, a case study applying these methods for the differentiation of polymorphs of bupivacaine HCl is also presented. All experiments were conducted upon samples with naturally-abundant nitrogen isotopes. For most of the APIs, it was possible to acquire frequency-stepped UW 14 N SSNMR spectra of stationary samples, which display powder patterns corresponding to pseudo-tetrahedral (i.e., RR'R"NH + and RR'NH 2 + ) or other (i.e., RNH 2 and RNO 2 ) nitrogen environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

State of knowledge and challenges of U-Si compounds for use in light water reactor accident tolerant fuel designs

Characterization of the properties of U-Si compounds first required synthesis of high purity material for each of the compositions. The four compounds targeted for investigation in this work were U{sub 3}Si, U{sub 3}Si{sub 2}, USi, and U{sub 3}Si{sub 5}. Specimens of U{sub 3}Si{sub 2}, U{sub 3}Si{sub 5}, and USi with specific geometries for individual testing procedures were prepared using a powder metallurgical method. Thermophysical properties of the U-Si compounds were determined within 100 K of their respective melt point or decomposition temperature. Thermal expansion was determined with a dilatometer, specific heat capacity by the ratio method in a differential scanning calorimeter using a sapphire standard, while thermal diffusivity was determined with a laser flash analyzer. Oxidation performance of the U-Si compounds was determined in a thermogravimetric analyzer (TGA), which measures the weight change of a sample as a function of gas composition and temperature. The results show that each of the U-Si compounds is electronically conductive leading to higher thermal conductivity values than the reference fuel UO{sub 2}. Higher thermal conductivity values will lead to enhanced safety margins within a reactor core and provide better economics over the lifetime of a fuel cycle. However, no improvements have been realized over the reference UO{sub 2} case with regards to oxidation performance in air although more testing is required to substantiate the differences especially in steam and corrosive aqueous LWR environments. Finally, there exists a lack of knowledge in the literature with regards to low burnup irradiation testing on all of the U-Si binary compounds, which would be necessary to simulate their performance in a reactor setting.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Asymmetric Cracking in Mar-M247 Alloy Builds During Electron Beam Powder Bed Fusion Additive Manufacturing

In the electron beam powder bed fusion (EB-PBF) process, a substantial number of high-gamma prime Ni-based superalloys are considered as non-printable due to a high propensity to form cracks. In this research, we focused on computational modeling framework to predict solidification-related cracking phenomena in EB-PBF processes. The cracking analysis was performed on cylindrical overhang structures where the cracks are observed only on one side of the part. Comprehensive microstructural characterization correlated the cracking tendency to low-melting point liquid-film formation along columnar grain boundaries with high misorientation angles due to partitioning of alloying elements. Uncoupled numerical thermal and mechanical models were used to rationalize the relationship between process parameters, build geometry, and cracking. The simulations showed asymmetric temperature distributions and associated asymmetric tensile thermal stresses over a cross section due to differences in section modulus and periodic changes in beam scanning directions. Here, the results provide a potential pathway based on spatially varying beam scanning strategies to reduce the cracking tendency during additive manufacturing of complex geometries on the overhang structure in high-gamma prime nickel-based superalloys.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Tensile Deformation of DED Graded IN718-René41 Superalloy at 650°C by in-situ Neutron Diffraction and Digital Image Correlation

A compositionally graded material comprised IN718 (718, γ'/γ" strengthened superalloy) and René41 (R41, a medium γ' strengthened superalloy) was fabricated using laser blown-powder directed energy deposition (DED/LB-M). Hot gas path components that require high and low temperature capabilities at different locations may benefit from such graded superalloy, potentially eliminating the use of welded or mechanically joined components and reducing cost. In the present work, microstructure and 650°C tensile behavior of 718-R41 graded superalloy in as-built and heat-treated states are investigated by Digital Image Correlation (DIC), in-situ neutron diffraction, coupled with conventional characterization techniques. The applied heat treatment generates static recrystallization and equiaxed grains in 718 rich compositions, while R41 rich compositions remain partially or un-recrystallized. Yield strengths of 718 and R41 sections in heat-treated state are comparable to wrought forms but the graded compositions show weakness. From neutron experiment, diffraction elastic constants and single crystal elastic constants are calculated, which show small difference between the as-built and heat-treated states and between the γ and γ' phases. Grain-level load transfer from the (220) grains to (200) grains is found to be composition dependent, and qualitatively agrees with DIC measured macroscopic yield strength. Within the (200) grains, the γ/γ' phases deform elastically until the γ phase yields and afterwards the γ' phase takes load from γ phase.

digital image correlation↗
DOE OSTI2019

Low-Temperature Rotational Tunneling of Tetrahydroborate Anions in Lithium Benzimidazolate-Borohydride Li 2 (bIm)BH 4

To investigate the dynamical properties of the novel hybrid compound, lithium benzimidazolate-borohydride Li 2 (bIm)BH 4 (where bIm denotes a benzimidazolate anion, C 7 N 2 H 5 - ), we have used a set of complementary techniques: neutron powder diffraction, ab initio density functional theory calculations, neutron vibrational spectroscopy, nuclear magnetic resonance, neutron spin echo, and quasi-elastic neutron scattering. Our measurements performed over the temperature range from 1.5 to 385 K have revealed the exceptionally fast low-temperature reorientational motion of BH 4 - anions. This motion is facilitated by the unusual coordination of tetrahedral BH 4 - anions in Li2(bIm)BH4: each anion has one of its H atoms anchored within a nearly square hollow formed by four coplanar Li+ cations, while the remaining -BH 3 fragment extends into a relatively open space, being only loosely coordinated to other atoms. As a result, the energy barriers for reorientations of this fragment around the anchored B-H bond axis are very small, and at low temperatures, this motion can be described as rotational tunneling. The tunnel splitting derived from the neutron spin echo measurements at 3.6 K is 0.43(2) ueV. With increasing temperature, we have observed a gradual transition from the regime of low-temperature quantum dynamics to the regime of classical thermally activated jump reorientations. The jump rate of the uniaxial 3-fold reorientations reaches 5 x 10 11 s -1 at 80 K. Nearer room temperature and above, both nuclear magnetic resonance and quasi-elastic neutron scattering measurements have revealed the second process of BH4- reorientations characterized by the activation energy of 261 meV. This process is several orders of magnitude slower than the uniaxial 3-fold reorientations; the corresponding jump rate reaches ~7 x 10 8 s -1 at 300 K.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Co/Cr co-doped MgGa{sub 2}O{sub 4} nanoparticles: Microstructure and optical properties

Graphical abstract: The Ga 2p{sub 3/2} spectra consist of two peaks, corresponding to Ga{sup 3+} ions placed at octahedral and tetrahedral sites, respectively. The fraction of tetrahedral Ga{sup 3+} ions (∼1117 eV) increases with increasing doping concentration. - Highlights: • Structural and properties of Co{sup 2+}/Cr{sup 3+}: MgGa{sub 2}O{sub 4} nanoparticles were characterized. • The distribution of cations was studied using XPS. • The inversion degree increased with increasing content of doping ions. • The doping concentration has also effect on absorption and emission properties. • Optical properties of nanoparticles were discussed based on the structural results. - Abstract: MgGa{sub 2}O{sub 4} nanoparticles co-doped with Co{sup 2+}/Cr{sup 3+} ions were prepared by a citrate sol–gel method. Their microstructure and optical properties were studied using X-ray powder diffraction (XRD), infrared spectroscopy, X-ray photoelectron spectroscopy (XPS), absorption and fluorescence spectroscopy. MgGa{sub 2}O{sub 4} nanoparticles with the size of 10–30 nm were obtained when the precursor was annealed at 800 °C. Results indicated that Ga{sup 3+} and Mg{sup 2+} cations occupied the octahedral sites as well as the tetrahedral sites in samples. The inversion degree of Ga or Mg increased with increasing content of doping ions. Absorption spectra indicated that Co{sup 2+} and Cr{sup 3+} ions entered both the tetrahedral and octahedral sites of spinel structure by substituting Mg{sup 2+} and Ga{sup 3+} ions, respectively. Emission spectra of the co-doped MgGa{sub 2}O{sub 4} showed a broad emission band peaking at 700 and 680 nm, relevant to the emission characteristic of octahedral Cr{sup 3+} and tetrahedral Co{sup 2+} ions.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Aerosol-Assisted Deposition for TiO 2 Immobilization on Photocatalytic Fibrous Filters for VOC Degradation

Atomization and spraying are well-established methods for the production of submicrometer- and micrometer- sized powders. In addition, they could be of interest to the immobilization of photocatalytic nanoparticles onto supports because they enable the formation of microporous films with photocatalytic activity. Here, we provide a comparison of aerosol-assisted immobilization methods, such as spray-drying (SD), spray atomization (SA), and spray gun (SG), which were used for the deposition of TiO 2 dispersions onto fibrous filter media. The morphology, microstructure, and electronic properties of the structures with deposited TiO 2 were characterized by SEM and TEM, BET and USAXS, and UV-Vis spectrometry, respectively. The photocatalytic performances of the functionalized filters were evaluated and compared to the benchmark dip-coating method. Our results showed that the SG and SA immobilization methods led to the best photocatalytic and operational performance for the degradation of toluene, whereas the SD method showed the lowest degradation efficiency and poor stability of coating. We demonstrated that TiO2 sprays using the SG and SA methods with direct deposition onto filter media involving dispersed colloidal droplets revealed to be promising alternatives to the dip-coating method owing to the ability to uniformly cover the filter fibers. In addition, the SA method allowed for fast and simple control of the coating thickness as the dispersed particles were continuously directed onto the filter media without the need for repetitive coatings, which is common for the SG and dip-coating methods. Our study highlighted the importance of the proper immobilization method for the efficient photocatalytic degradation of VOCs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Grain structure and texture selection regimes in metal powder bed fusion

Additive manufacturing (AM) offers opportunities to produce complex part geometries not possible with conventional processing and in some cases even improve part performance. However, adoption has been slowed by difficulties assessing microstructure variability and there is no straightforward approach to relate processing to grain structure characteristics. In this study, datasets from AdditiveFOAM heat transport simulations of laser powder bed fusion (LPBF) are used to drive ExaCA simulations of grain structure. The GPU utilization of ExaCA and an algorithmic update for modeling melt pool overlap region solidification enabled rapid and parallel simulation across a wider range of process conditions than previously explored with cellular automata-based solidification models. A texture selection angle $θ_s$ is defined based on melt pool overlap geometry, and the range of $θ_s$ over which a commonly observed texture transition occurs in characterized AM builds was well-reproduced by ExaCA simulations over a wide range of melt pool shape, hatch spacing, and layer height. ExaCA simulations with 90 degree rotation of the scan direction on every other layer reproduced a number of trends from the AM literature including grain refinement, the dominance of layers with larger melt pools on the final grain structure, and the weakening or strengthening of texture depending on odd and even layer melt pool overlap geometry. EBSD data from a benchmark AM part is used to validate the simulated mechanism of a layer rotation-induced texture strengthening effect. Importantly, these results expand the understanding of the mechanisms for texture selection in alloys with cubic crystal symmetry and offer an approach to easily evaluate processing conditions. With this new understanding, these modeling tools will enable anticipation of previously unexpected variations in grain structure and target specific microstructures and properties.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Fabrication of yeast engineered porous 13X adsorbent layers for CO 2 capture

This study investigates a novel environmentally friendly coating technique using yeast fermentation to obtain super porous Zeolite 13X adsorbent layers through freeze-drying technique for CO 2 capture applications. Several mass ratios of sugar to yeast were used to control the porosity and pore sizes in the adsorbent layer. A unique peeling process was integrated to obtain foamy, hollow structures to have deeper layer accessibility of adsorbent for adsorption applications. These coated adsorbent layers were experimentally characterized as a function of the mass ratio of sugar to yeast and adsorbent solid fraction. Scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), and Fourier-transform infrared spectroscopy (FT-IR) are used to analyze the coated layers. Here, the void fraction for coated samples is found to vary between 0.48 and 0.56, making the samples applicable for adsorption applications. Adsorption performance experiments are performed to test the coated samples' performance compared to 13X powder. Due to their simplistic fabrication, cost-effectiveness, rapid pore formation, and high adsorption capacity, these porous 13X layers hold potential for large-scale fabrication and CO 2 capture applications.

Adsorbent coating↗
DOE OSTI2018

Microstructural characterization and comparison of Ti-6Al-4V manufactured with different additive manufacturing processes

In this work, the microstructures of Ti-6Al-4V manufactured by different additive manufacturing (AM) processes have been characterized and compared. The microstructural features that were characterized are the α lath thickness, grain boundary α (GB-α) thickness, prior β grain size and α colony size. In addition, the microhardnesses were also measured and compared. The microstructure of shaped metal deposited (SMD) Ti-6Al-4V material showed the smallest variations in α lath size, whereas the material manufactured with laser metal wire deposition-0 (LMwD-0) showed the largest variation. The prior β grain size was found to be smaller in material manufactured with powder bed fusion (PBF) as compared with corresponding material manufactured with the directed energy deposition (DED) processes. Parallel bands were only observed in materials manufactured with DED processes while being non-present in material manufactured with PBF processes.

36 MATERIALS SCIENCE↗
DOE OSTI2016

The effect of diameter ratio between transducers and reactor in sonication-assisted synthesis of Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} nanoparticles

This paper describes the particle size characterization of mechanically alloyed Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} prepared with the aid of a high-power ultrasonic destruction. Analytical-grade BaCO{sub 3}, TiO{sub 2} and SrCO{sub 3} with a purity greater than 99 wt.% were used as precursors for Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3}. The mechanically powders were respectively sintered at 1200 °C for 3 hours to form crystalline powders. This work is aimed at studying the effect of diameter ratio between reactor and transducer of a high power sonicator on the Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} nanoparticles formation. The presence of a single phase of the two materials was confirmed by X-Ray Diffraction (XRD). The concentration of the particles in demineralized water was 3.0 g / 100 mL which become the object of 3 hours ultrasonic destruction subjected to the application of transducer in which the ratio between the diameter of the reactor and the transducer (D/d) was fixed at 1.4, 1.6 and 1.8 respectively. It was found that the mean particle size before the ultrasonic destruction was 538 nm for Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and 480 nm for Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3}. With D/d of 1.8, the mean particle size of the two materials was found to decrease drastically to 38 nm and 24 nm, respectively. These mean particle sizes were respectively comparable with that of the crystallite size of the particles derived using the Whole Powder Pattern Modelling (WPPM) from which the mean crystallite size of 22 nm for Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and 14 nm for Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} were obtained. It is then confirmed single nanocrystallite Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} and Ba{sub 0.3}Sr{sub 0.7}TiO{sub 3} particles were already achieved. We can conclude that the ultrasonic destruction to mechanically milled crystalline particles would be one of an effective way to produce nanoparticles.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2025

Synthesis and Characterization of Metastable Cobalt Honeycomb KCoAsO 4

The Kitaev model has served as a long-sought-after target in the realization of a quantum spin liquid that could host Majorana Fermions. Such non-Abelian anyons could revolutionize quantum computing if properly implemented to overcome decoherence. A 3d 7 electronic configuration, like Co 2+ , has been explored by theory and experimental work to design Kitaev materials. Here, in this study, we report the synthesis of a new cobaltate honeycomb material KCoAsO 4 . The compound is synthesized through a low-temperature solution route and crystallized in space group R¯3 with lattice parameters a = 5.0394(1) and c = 28.6790(1) as determined by neutron powder diffraction. The crystal structure follows motifs similar to those of the honeycomb compound BaCo2(AsO 4 ) 2 but presents differing magnetic behavior. Magnetization/heat capacity measurements on the powder show antiferromagnetic transition T N = 14 K. Two lower-temperature transitions are present in susceptibility at low field that resemble spin reorientations. Magnetization data as a function of field have curvature indicative of metamagnetic behavior below the magnetic ordering temperature, with the magnetic ordering suppressed upon application of a higher magnetic field. Computational studies suggest the presence of a weak nearest-neighbor Kitaev term, K 1 , consistent with related honeycomb cobaltates. Together, the data suggest that this material should present a new platform for developing Kitaev quantum spin liquids.

cobaltate↗
DOE OSTI2018

Interaction between laser radiation and metallic powder of 316L austenitic steel during selective laser melting

Highlights: • Single and multiple tracks on a loose bulk powder substrate were generated. • Understanding of the microstructure development during SLM was achieved. • Single tracks reveal a nearly symmetrical crystallography with elongated grains. • Multiple tracks show elongated grains perpendicular to the build direction. - Abstract: During selective laser melting (SLM), a complex heat state develops that leads to a characteristic crystallography and microstructure of the processed materials. Depending on the geometry of the processed part, most scan tracks of a new layer, so-called hatches, are located above a dense substrate or already solidified structures whereas others are located above loose powder. This is, inter alia, the case for overhanging structures. Attributable to the lower thermal conductivity of loose powder, temperature gradients and cooling rates of the melt pool differentiate in these areas, resulting in a different microstructural build-up. In this work, the microstructure and the crystallographic orientation of grade 316L austenitic stainless steel processed by SLM was investigated to understand the interaction between the laser radiation and the metallic powder during SLM-processing and to investigate the remelting of a track on a previous SLM-densified track. Single and multiple tracks on a loose bulk powder substrate, as well as single tracks on a dense substrate plate, were generated. A parameter study revealed that high energy densities are necessary to build continuous tracks on a loose bulk powder substrate. In addition, the amount of adhered particles, which are sintered on the fully melted and solidified tracks, is determined in comparison to the melted powder because the sintered particles strongly influence the surface roughness. To understand the microstructure development and, particularly, the influence of adjacent hatches during SLM-processing, investigations on the resulting microstructure and crystallographic orientation of a single track and two connected multiple tracks were carried out. During SLM processing of the tracks, the substrate plate and the solidified structures influence the temperature gradient and cooling rate of the melt pool, thus directionally solidified and elongated grains occur. Furthermore, the solidification is characterized by an epitaxial growth due to a distinct thermal gradient between the melt pool and the surrounding elements.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Synthesis, characterization and electrocatalytic properties of delafossite CuGaO{sub 2}

Delafossite CuGaO{sub 2} has been employed as photocatalysts for solar cells, but their electrocatalytic properties have not been extensively studied, especially no comparison among samples made by different synthesis routes. Herein, we first reported the successful synthesis of delafossite CuGaO{sub 2} particles with three different morphologies, i.e. nanocrystalline hexagons, sub-micron sized plates and micron–sized particles by a modified hydrothermal method at 190 °C for 60 h [1–3], a sono-chemical method followed by firing at 850 °C for 48 h, and a solid state route at 1150 °C, respectively. Morphology, composition and phase purity of the synthesized samples was confirmed by powder X-ray diffraction and Raman spectroscopic studies, and then their electrocatalytic performance as active and cost effective electrode materials to the oxygen and hydrogen evolution reactions in 0.5 M KOH electrolyte versus Ag/AgCl was investigated and compared under the same conditions for the first time. The nanocrystalline CuGaO{sub 2} hexagons show enhanced electrocatalytic activity than the counterpart sub-micron sized plates and micron-sized particles. - Graphical abstract: Representative delafossite CuGaO2 samples with sub-micron sized plate and nanocrystalline hexagon morphologies accompanying with chronoamperometric voltammograms for oxygen evolution reaction and hydrogen evolution reaction in 0.5 M KOH electrolyte after purged with N{sub 2} gas. - Highlights: • Delafossite CuGaO{sub 2} with three morphologies has been synthesized. • Phase purity of the synthesized samples was confirmed. • Comparison on their electrocatalytic properties was made for the first time. • Their use as electrodes for oxygen and hydrogen evolution reactions was evaluated. • Nanocrystalline CuGaO{sub 2} hexagons show highest electrocatalytic activity.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Fabrication and characterization of multifunctional Fe/TiO2 composite coatings

Highlights: • Electrodeposition of Fe/TiO{sub 2} composite coatings using methanesulfonate electrolytes. • TiO{sub 2} sol is synthesized by means of precipitation technique. • Electrodeposition kinetics obeys the improved Guglielmi's model. • Incorporation of TiO{sub 2} into Fe matrix results in an increase in microhardness. • Enhanced electrocatalytic and photocatalytic activity of Fe/TiO{sub 2} composites. - Abstract: Composite Fe/TiO{sub 2} coatings were electrodeposited using environmentally friendly colloidal methanesulfonate electrolytes. A sol of titania nano-particles was synthesized by means of precipitation technique. The electrodeposition parameters and the properties of composite coatings were compared with those typical of analogous composite electrodeposits produced from the plating bath containing suspended commercially available nano-powder Degussa P25. The electrodeposition process obeys the modified Guglielmi's model. The incorporation of TiO{sub 2} dispersed phase into iron matrix results in an appreciable increase in the microhardness due to dispersion strengthening. The microhardness of deposits obtained from electrolyte with the addition of nano-sized titania sol exceeds that which is observed for coatings produced from the bath containing aggregated Degussa P25 TiO{sub 2} particles. The introduction of dioxide titanium particles into Fe matrix yields photocatalytic properties towards the reaction of organic dye degradation and improves electrocatalytic performance towards hydrogen and oxygen evolution reactions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Bulk nanocrystalline Al–Mg–Y alloys with amorphous grain boundary complexions display high strength and compressive plasticity

Although nanocrystalline alloys regularly exhibit high strengths, their use in structural applications often face challenges due to sample size limitations, unstable microstructures, and the limited ability to plastically deform. The incorporation of amorphous grain boundary complexions has been proposed to address these issues, by simultaneously stabilizing nanocrystalline grain structures for scale-up processing and improving alloy toughness. In the present study, the mechanical behavior of bulk nanocrystalline Al–Mg–Y is examined with macroscale compression testing, probing a length scale that is relevant to real-world structural applications. Bulk samples were fabricated via a simple powder metallurgy approach, with different hot-pressing temperatures and durations employed for consolidation in order to investigate microstructural and property evolution. All of the specimens contained primary face-centered cubic Al and secondary Al 4 C 3 and Al 3 Y phases, with the Al 3 Y particles exhibiting two populations of small equiaxed and larger elongated particles. Appreciable plasticity was measured along with high ultimate stresses over 800 MPa due to the presence of amorphous grain boundary complexions. Microstructural characterization of fracture surfaces revealed that the area fraction of dimpled regions increased with longer hot-pressing time. Most importantly, the elongated Al 3 Y particles formed regular cellular patterns with increasing hot-pressing time, delaying shear localization and significantly enhancing plasticity. The hierarchy present in the microstructure of the Al–Mg–Y alloy, from amorphous grain boundary complexions to secondary phases, gives rise to excellent bulk mechanical properties, which are attractive for structural applications.

Bulk nanocrystalline alloy↗