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At least 1,567 records · Page 87
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Influence of Thermomechanical Treatment on Structural-Phase Transformations and Mechanical Properties of the Cu–Al–Ni Shape-Memory Alloys

Using the methods of optical and electron microscopy and electron and X-ray diffraction analyses, the influence of thermomechanical treatment on the mechanical properties, average grain size, and structural and phase transformations is investigated in the Cu–Al–Ni triple alloys exhibiting a shape memory effect. In the alloys under study with a fixed content of 3wt% Ni the concentration of aluminum was varied from 9 to 14 wt%. It is shown that in the alloys subjected to thermal treatment, including forging and homogenizing annealing using controlled recrystallization in the austenitic state followed by quenching, the grain-boundary disintegration and segregation disappear. It is found out that the microstructure of the alloys in the hot-forged and hardened states with the content of aluminum 9–10 wt%. consists of the grains of the average dimensions within 60–80 μm, with the content of aluminum 10–12 wt% – 100–350 μm, while in the alloys with the content of aluminum up to 14 12 wt% the average grain size reaches 1 mm. According to the data of mechanical testing at room temperature, with a decrease in the content of aluminum the ultimate tensile strength (σ{sub UTS}), the yield strength (σ{sub М}) and the relative elongation (δ) increase. An improvement of the mechanical properties of the alloys is attributed to the grain structure refinement of the β{sub 2}-austenite and package substructure of the β'{sub 1}-and γ'{sub 1}-martensites as the content of aluminum in the alloys decreases. For instance, in the fine-grained alloys containing 9.2 and 9.5 wt% Al the value of relative elongation remains at a high level (>10%), while for the other alloys with 10–14 wt% Al it does not exceed 5%. As the content of aluminum in the alloys decreases, the character of the specimen fracture under uniaxial tension changes (from brittle to ductile).

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2015

Analysis of integrity and microstructure of linear friction welded Waspaloy

Nickel-base superalloy, Waspaloy, was linear friction welded (LFWed) under different axial shortening conditions of 2.0, 3.4, and 4.6 mm. The tensile properties and microhardness of the weldments were investigated in the as-LFWed condition and compared with those in the post-weld heat treated (PWHTed) condition. Mechanical properties were related to microstructures following examination by optical microscopy, high resolution scanning electron microscopy, and electron backscatter diffraction (EBSD). Analyses of the EBSD results in terms of the misorientation angle distribution, which represents the stored energy, were performed. In the as-LFWed condition, the yield strength (YS) and ultimate tensile strength (UTS) increased with axial shortening due to greater expulsion of the softened interfacial material toward the periphery as flash. In contrast, with increasing axial shortening the total elongation initially remained constant and then decreased. This was also related to the expulsion of the softened interfacial material into the bifurcated flash. Extensive dissolution of the strengthening phase (γ′) in the weld area during linear friction welding (LFW) contributed to the lower YS and UTS in the as-welded condition compared to the PWHTed condition where the γ′ particles were recovered. After performing post-weld heat treatment (PWHT), the total elongation improved due to the relaxation of stored energy and grain growth in the thermomechanically affected zone (TMAZ). - Highlights: • Tensile property and microstructure in Waspaloy linear friction welds were studied. • Yield strength and ultimate tensile strength increased with axial shortening. • Elongation initially remained constant and then decreased with axial shortening. • Post-weld heat treat recovered dissolved γ′ particles and increased weld strength. • Stored energy relaxation during post-weld heat treatment improved weld elongation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Effect of gadolinium addition on microstructural evolution and solidification characteristics of Al-15%Mg2Si in-situ composite

Highlights: • The Al{sub 3}Gd is the heterogeneous nucleation of primary Mg{sub 2}Si in Al-15%Mg{sub 2}Si composite. • Addition of Gd to Al-15%Mg{sub 2}Si resulted in the formation of Al{sub 2}Si{sub 2}Gd and AlSiGd intermetallic compounds. • Absorption of Gd atoms preferentially on {100} facets of Mg{sub 2}Si crystals changed its growth manners. • Primary Mg{sub 2}Si transformed from coarse-dendritic to perfect truncated octahedral shape after treating with 1.0 wt% Gd. • Gd addition increased the nucleation and growth temperatures of primary Mg{sub 2}Si. - Abstract: The current study investigated the effects of gadolinium (Gd) addition (0, 0.3, 0.5, 1.0, and 2.0 wt%) on microstructural development and solidification characteristics of hypereutectic Al-15%Mg{sub 2}Si in-situ composite. Microstructural examinations were carried out via optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD), transmission electron microscopy (TEM), and electron backscattered diffraction (EBSD). The results showed that an addition of 1.0 wt% Gd, changed the morphology of primary Mg{sub 2}Si from coarse dendritic to fine truncated octahedral shape. Furthermore, the average size of primary Mg{sub 2}Si particles decreased from 40 μm to 20 μm and density increased from 495 to 1167 particles/mm{sup 2}. Besides that, cooling curve thermal analysis (CCTA) technique revealed that Gd addition increased nucleation and growth temperatures of primary Mg{sub 2}Si phase. It is proposed that modification and refinement mechanism of Gd addition are mainly attributed to formation of tiny Al{sub 3}Gd particles as the heterogeneous nucleation substrates for primary Mg{sub 2}Si, which results in a refined distribution of these particles and poisoning effect by adsorbing Gd atoms, preferentially on {100} facets of Mg{sub 2}Si crystals. Moreover, it is believed that formation of Gd intermetallic compounds is responsible for refinement of primary Mg{sub 2}Si particles.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Evaluation of the microstructure and mechanical properties of WC particle reinforced aluminum matrix composites fabricated by friction stir processing

Highlights: • FSP was used for the preparation of aluminum matrix composites reinforced with WC particle. • WC particles were uniformly distributed in the composite. • WC particles refined the grains of aluminum matrix. • WC particles enhanced the hardness and tensile strength, but decreased the ductility. - Abstract: Tungsten carbide (WC) is an attractive reinforcing material for aluminum and its alloys. However, it is technically challenging to fabricate WC particle reinforced aluminum matrix composites (AMCs) with homogeneous distribution of WC particles by liquid state processing techniques because of large density gradient. The present work aim to produce WC particle reinforced aluminum matrix composites (AMCs) through friction stir processing (FSP) and analyze the effect of its volume fraction on the microstructural features and the mechanical behavior of the developed AMCs. Microstructural evaluation was conducted on the cross-sections of the samples by optical microscopy (OM), scanning electron microscopy (SEM) and electron backscattered diffraction (EBSD). Microhardness testing was conducted across the cross-sections of FSPed samples to obtain hardness profiles and tensile test was conducted on as-received Al and FSPed samples. The fabricated AMCs exhibited the homogeneous distribution of WC particle with no obvious particle clustering in the stir zone, irrespective of position and WC particle volume fraction. Excellent WC/Al interfacial bonding was obtained in all FSPed AMCs with obviously refined grains. The average size of WC particles after FSP was slightly reduced with the increased volume fraction. It was also found that increasing the volume fraction of WC particles favored the grain refinement, improved the hardness and strength, but decreased the ductility. This improvement in the hardness and strength was attributed to the grain refinement strengthening and homogeneous distribution of WC particles. The decreased ductility resulted from the introduction of more WC particles. Increasing the volume fraction of WC particles caused the nature of fracture to move towards brittle nature.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Pulsed laser powder bed fusion additive manufacturing of A356

Highlights: • Dense A356 specimens (98 ± 0.4%) were fabricated using a customized P-LPBF system. • Microstructure and grain morphology were examined using LOM, SEM, and EBSD. • Solidification front velocities (R) were evaluated through the KGT model. • A columnar grain structure was observed and predicted by the Hunt's criterion. - Abstract: A356 (Al7SiMg) specimens were fabricated through pulsed laser powder bed fusion (P-LPBF) additive manufacturing. Microstructural examinations and analyses were carried out through the usage of light optical microscopy (LOM), scanning electron microscopy (SEM), and electron backscatter diffraction (EBSD). The results revealed a fine cellular microstructure with the intercellular network consisting of Al cells and defined by a network of Si arms. The Al cells at the center of the melt pools and within the melt pool boundary bands were measured to be 423 ± 49 nm and 664 ± 76 nm, respectively. The presence of a fine columnar grain structure and epitaxial growth on partially melted grains was observed and explained by the KGT model and Hunt's criterion.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Effect of oxygen partial pressure on microstructural and optical properties of titanium oxide thin films prepared by pulsed laser deposition

Graphical abstract: - Highlights: • Microstructural and optical properties are studied systematically. • The optical properties are studied by UV–visible and photoluminescence. • The PL spectra shows two peaks correspond to bandgap of anatase and rutile. • The maximum refractive index of 2.73 is obtained for rutile phase of titania. - Abstract: Nanocrystalline titanium oxide (TiO{sub 2}) thin films were deposited on silicon (1 0 0) and quartz substrates at various oxygen partial pressures (1 × 10{sup −5} to 3.5 × 10{sup −1} mbar) with a substrate temperature of 973 K by pulsed laser deposition. The microstructural and optical properties were characterized using Grazing incidence X-ray diffraction, atomic force microscopy, UV–visible spectroscopy and photoluminescence. The X-ray diffraction studies indicated the formation of mixed phases (anatase and rutile) at higher oxygen partial pressures (3.5 × 10{sup −2} to 3.5 × 10{sup −1} mbar) and strong rutile phase at lower oxygen partial pressures (1 × 10{sup −5} to 3.5 × 10{sup −3} mbar). The atomic force microscopy studies showed the dense and uniform distribution of nanocrystallites. The root mean square surface roughness of the films increased with increasing oxygen partial pressures. The UV–visible studies showed that the bandgap of the films increased from 3.20 eV to 3.60 eV with the increase of oxygen partial pressures. The refractive index was found to decrease from 2.73 to 2.06 (at 550 nm) as the oxygen partial pressure increased from 1.5 × 10{sup −4} mbar to 3.5 × 10{sup −1} mbar. The photoluminescence peaks were fitted to Gaussian function and the bandgap was found to be in the range ∼3.28–3.40 eV for anatase and 2.98–3.13 eV for rutile phases with increasing oxygen partial pressure from 1 × 10{sup −5} to 3.5 × 10{sup −1} mbar.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Quasi-static and dynamic response of a Cu/Nb composite following equal channel angular extrusion

The article presents a study of the plastic properties of a Cu–18%Nb composite following equal channel angular extrusion under both low- and high-strain rate loadings. The microstructures are characterized by optical and scanning electron microscopy as well as electron backscatter diffraction. Comparisons are also made with a Cu–50%Nb laminate made by accumulative roll bonding. Textures obtained within the respective phases in the extruded composite closely mimic those previously reported for the pure components alone (Cu, Nb). Grain sizes of the major phase (Cu) exhibit broad distributions, due largely to partial recrystallization during the extrusion process. Further re-crystallization is obtained within localized deformation bands produced at high strain rates (3 × 10 3 s –1 ). While the degree of anisotropy and the strain rate sensitivity of the composite response are similar to those of pure Cu after extrusion, the strength levels of the composite are somewhat greater, falling broadly between those obtained in the pure components after extrusion to comparable plastic strains. Furthermore, the implications for selection of composite composition and processing for achieving higher strengths are briefly discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Structure–property relations in graphitic pebbles for nuclear applications

This work presents an analytical approach for holistically characterizing graphitic matrix pebbles for nuclear applications whereby the macrostructure, microstructure, and thermophysical properties of pebbles are determined. A systematic sectioning method was applied to several pebbles to describe the regional properties of the samples. Intact matrix-only spheres and sections of spheres fabricated by Kairos Power were characterized via optical imaging, x-ray computed tomography, x-ray diffraction, and ellipsometry to determine 2D and 3D macrostructure and anisotropy. The thermophysical properties of these materials were determined via measurements of density, specific heat, thermal expansion, and thermal diffusivity. The results of this study indicate that the pebble fabrication methods and their resultant effect on microstructure have a nontrivial effect on thermophysical properties, confirming the importance of robust characterization of these components. A discussion of the characterization approach and its applicability to nuclear fuel development activities is also included.

42 ENGINEERING↗
DOE OSTI2024

Chlorfenapyr Crystal Polymorphism and Insecticidal Activity

Four crystalline polymorphs of the proinsecticide chlorfenapyr [4-bromo-2-(4-chlorophenyl)-1-ethoxymethyl-5-trifluoromethyl-1H-pyrrole-3-carbonitrile] have been identified and characterized by polarized light optical microscopy, differential scanning calorimetry, Raman spectroscopy, X-ray diffraction, and electron diffraction. Three of the four structures were considered polytypic. Chlorfenapyr polymorphs show similar lethality against fruit flies (Drosophila melanogaster) and mosquitoes (Anopheles quadrimaculatus) with the least stable polymorph showing slightly higher lethality. Similar activities may be expected to be consistent with structural similarities. Knockdown kinetics, however, depend on an internal metabolic activating step, which further complicates polymorph-dependent bioavailability.

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

Probing the Crystal Structure and Formation Mechanism of Lanthanide-Doped Upconverting Nanocrystals

Lanthanide (Ln)-doped upconverting nanocrystals (UCNCs), such as NaLnF 4 (with Ln = lanthanide), constitute an important class of nanoscale materials due to their capacity to convert near-infrared photons into near-ultraviolet or visible light. Although under intense investigation for more than a decade, UCNCs have been relatively underexplored especially regarding their crystal structure and mechanisms of formation in organic media. The former is needed to explain the relationship between atomic scale structure and upconversion (UC) properties of UCNCs (i.e., local symmetry for 4f–4f transition probability, Ln 3+ distances for energy migration), while the latter is essential to finely tune the size, morphology, chemical composition, and architecture of well-defined upconverting nanostructures, which constitute the experimental levers to modify the optical properties. In this contribution, we use synchrotron-based diffraction experiments coupled to Rietveld and pair distribution function (PDF) analyses to understand the formation of NaGdF 4 :Yb:Er UCNCs in organic media and to investigate their crystal structure. Our results reveal a complex mechanism of the formation of NaGdF 4 :Yb:Er UCNCs based on chemical reactions involving molecular clusters and in situ-generated, crystalline sodium fluoride at high temperature. Additionally, a detailed crystallographic investigation of NaGdF 4 :Yb:Er UCNCs is presented. Our Rietveld and PDF analyses show that the space group P$\bar{6}$ is the one that best describes the crystal structure of NaGdF 4 :Yb:Er UCNCs contrary to what has been recently proposed. Further, our Rietveld and PDF data reveal the formation of bulk-like crystal structure down to 10 nm with limited distortions. Finally, the results presented in this paper constitute an important step toward the comprehensive understanding of the underlying picture that governs UC properties of lanthanide-doped nanostructures.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

High-Pressure Investigation of 2,4,6-Trinitro-3-bromoanisole (TNBA): Structural Determination and Piezochromism

Understanding phase transitions in energetic materials is crucial for developing predictive models of detonation. 2,4,6-Trinitro-3-bromoanisole (TNBA), an energetic material, was studied in its single-crystal form up to pressures of 45 GPa in a diamond anvil cell. The material was characterized by using X-ray, Raman, and optical transmission measurements. From single-crystal X-ray diffraction, the ambient structure of TNBA was determined which crystallizes in the P2 1 /c space group having four molecular units per unit cell. The X-ray data up to 9.2 GPa were fitted to a third-order Birch–Murnaghan equation of state by using the parameters K o = 13.2(2.4) GPa and K p = 5.1(1.4). Between 6.8 and 7.3 GPa, a phase transition was inferred in TNBA from concurrent fading of X-ray diffraction, disappearance of Raman peaks, increase in sample fluorescence, and discontinuous color change. The new phase was consistent with an amorphous state of at least partially intact molecules judging from the presence of higher-order Raman modes and irreversibility of the Raman spectra upon release. Piezochromism was observed with the translucent yellow TNBA gradually darkening and becoming opaque black at ~25 GPa. This correlated to the absorption edge gradually shifting to the red in the visible spectrum. Signs of two possible additional structural transitions were detected in the 32.4–41.0 GPa range as suggested by a jump in the absorption edge, the irreversible changes in the absorption spectrum upon release to ambient pressure, and by the lack of Raman modes in recovered samples. Here, the crystal and electronic structures of TNBA were also investigated up to 10 GPa by using DFT calculations and crystal structure prediction (CSP) simulations. In agreement with the experimentally observed transition at 7 GPa, the simulations at 10 GPa found a bevy of polymorphs lower in enthalpy and higher in density than P2 1 /c. The lowest calculated enthalpy structure was determined to be P2 1 2 1 2 1 , being in a different space group than the ambient experimental result.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Examining Metal Identity and Proximity Effects on Acetylene Hydrogenation with Azolate-Based MOFs

Liquid organic hydrogen carriers (LOHCs) are an attractive fuel source due to their compatibility with existing transportation methods and ease of use. However, they suffer from sluggish (de)hydrogenation kinetics. One promising platform for developing next-generation catalysts is metal–organic frameworks (MOFs), which can enable systematic interrogation into the influence of metal identity and spatial arrangement. In this study, the effect of the coordination environment was investigated using Ni- and Co-based azolate MOFs: MFU-4l-OH (M x Zn 5–x (OH) 4 (BTDD) 3 ; x = 4 for M = Co and x = 3 for M = Ni, H 2 BTDD = bis(1H-1,2,3-triazolo[4,5-b][4′,5′-i])dibenzo[1,4]dioxin), composed of single-site nodes, and M(OH) 2 BBTA (M = Ni, Co; H 2 BBTA = 1H,5H-benzo(1,2-d:4,5-d’)bistriazole), composed of extended chain-type nodes. The catalysts were characterized by isotherms, powder X-ray diffraction (PXRD), scanning electron microscopy (SEM), inductively coupled plasma-optical emission spectroscopy (ICP-OES), and X-ray photoelectron spectroscopy (XPS) analysis. Acetylene hydrogenation activity under steady state conditions (150 °C, 1:1 C 2 H 2 :H 2 ) revealed higher turnover frequencies (TOFs) up 1.17 × 10 –2 mol C 2 H 2 mol −1 Ni min −1 and 1.98 × 10 –3 mol C 2 H 2 mol −1 Co min −1 for Ni-MFU-4l-OH and Co-MFU-4l-OH, respectively, compared to their BBTA analogues. However, the Co-based MOFs, particularly Co 2 (OH) 2 -BBTA, exhibited greater selectivity (up to 19%) for the fully hydrogenated ethane product. Isosteric heat of adsorption (Q st ) measurements for ethylene and ethane revealed that the BBTA framework had stronger binding to the products than MFU-4l. Furthermore, these findings demonstrate that metal identity and coordination environment may modulate acetylene hydrogenation performance, leading to design principles for tuning LOHC hydrogenation catalysts.

catalysts↗
DOE OSTI2013

Magnetic-field annealing of inverted polymer:fullerene hybrid solar cells with FePt nanowires as additive

We demonstrate a facile annealing method to improve the polymer chain ordering of poly(3-hexythiophene) (P3HT):fullerene blend triggered by a small amount of FePt nanowires (FePt NWs). By applying a magnetic field perpendicular to the substrate during the solvent drying process, the resulting P3HT:fullerene:FePt NWs film becomes highly optical anisotropy and exhibits a much stronger X-ray diffraction intensity of P3HT. We hypothesize that the coupling force between the FePt NWs and P3HT can assist the polymer chain alignment leading to an improved device performance. The proposed approach is simple and can be applied to other polymer blend systems as well.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2014

Zonal wavefront estimation using an array of hexagonal grating patterns

Accuracy of Shack-Hartmann type wavefront sensors depends on the shape and layout of the lenslet array that samples the incoming wavefront. It has been shown that an array of gratings followed by a focusing lens provide a substitution for the lensslet array. Taking advantage of the computer generated holography technique, any arbitrary diffraction grating aperture shape, size or pattern can be designed with little penalty for complexity. In the present work, such a holographic technique is implemented to design regular hexagonal grating array to have zero dead space between grating patterns, eliminating the possibility of leakage of wavefront during the estimation of the wavefront. Tessellation of regular hexagonal shape, unlike other commonly used shapes, also reduces the estimation error by incorporating more number of neighboring slope values at an equal separation.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2015

Zn interstitial defects induced magnetic nature in Fe ions doped ZnO based DMS

This paper describes the synthesis of Fe doped ZnO samples Zn{sub 1-x}Fe{sub x}0, where x various from 0.01≤x≤0.05 (in steps of 0.01) by solution method. The effect of Fe ions doping on the structural, optical and magnetic properties was investigated using X-ray diffraction (XRD), Photoluminescence and vibrating sample magnetometer (VSM) measurements. The observed result indicates that the samples are single phase formation of the wurtzite structure without any significant secondary phase in it. The photoluminescence spectra reveals the presence of Zn vacancies. The magnetic property of prepared samples was studied using a vibrating sample magnetometer and the observed results revealed a super-paramagnetic behavior for the Fe doped ZnO samples.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Preparation and characterization of PVP-PVA–ZnO blend polymer nano composite films

Flexible self-standing films of PVP-PVA blend composites are prepared by using ZnO as a nano filler at different concentrations. The structural, compositional, morphological and optical studies made with the help of X-ray diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Scanning electron microscope (SEM), Atomic Force Microscopy (AFM), Ultraviolet-visible spectroscopy (UV-vis) and Photoluminescence (PL) spectra are presented in this paper. The results of XRD indicate that ZnO nanoparticles are formed with hexagonal phase in the polymeric matrix. SEM images show the dispersion of ZnO nano filler in the polymer matrix. UV–vis spectra reveal that the absorption peak is centered around 235 nm and 370 nm for the nano composite films. The blue shift is observed with decrease in the concentration of the nano filler. PL spectra shows the excitation wavelength is given at 320 nm.The emission peaks were observed at 383 nm ascribing to the electronic transitions between valence band and conduction band and the peak at 430 nm.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Cross-coupled composite-cavity organic microresonators

We report on cross-coupled composite-cavity microresonators consisting of a vertical cavity and a second-order distributed feedback structure which employ the same organic active medium and support surface-normal and in-plane emission at the same time. The optical coupling is due to a first-order light diffraction on a second-order Bragg grating and, in the degenerate case, can be as efficient as the coupling observed in more classical cascade coupled cavities. When the system is non-degenerate, the diffraction efficiency is suppressed because of sub-coherence-length dimensions of the composite-cavity and both resonators tend to operate as independent structures without experiencing substantial losses due to diffraction on the distributed-feedback grating.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗