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At least 685 records · Page 38

Evolution of magnetic properties and microstructure of Hf{sub 2}Co{sub 11}B alloys

Amorphous Hf{sub 2}Co{sub 11}B alloys produced by melt-spinning have been crystallized by annealing at 500–800 °C, and the products have been investigated using magnetization measurements, x-ray diffraction, and scanning electron microscopy. The results reveal the evolution of the phase fractions, microstructure, and magnetic properties with both annealing temperature and time. Crystallization of the phase denoted HfCo{sub 7}, which is associated with the development of coercivity, occurs slowly at 500 °C. Annealing at intermediate temperatures produces mixed phase samples containing some of the HfCo{sub 7} phase with the highest values of remanent magnetization and coercivity. The equilibrium structure at 800 °C contains HfCo{sub 3}B{sub 2}, Hf{sub 6}Co{sub 23}, and Co, and displays soft ferromagnetism. Maximum values for the remanent magnetization, intrinsic coercivity, and magnetic energy product among the samples are approximately 5.2 kG, 2.0 kOe, and 3.1 MGOe, respectively, which indicates that the significantly higher values observed in crystalline, melt-spun Hf{sub 2}Co{sub 11}B ribbons are a consequence of the non-equilibrium solidification during the melt-spinning process. Application of high magnetic fields during annealing is observed to strongly affect the microstructural evolution, which may provide access to higher performance materials in Zr/Hf-Co hard ferromagnets. The crystal structure of HfCo{sub 7} and the related Zr analogues is unknown, and without knowledge of atomic positions powder diffraction cannot distinguish among proposed unit cells and symmetries found in the literature.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Dynamic shear localization of a titanium alloy under high-rate tension characterized by x-ray digital image correlation

Highlights: • First systematic error analyses for XDIC • First XDIC study of Ti-6Al-4V under dynamic tension • Deformation mode transition induces dynamic ductility decrease. • Dynamic shear localization due to rate-dependent microvoid coalescence process. - Abstract: Dynamic and quasi-static tension experiments are conducted on Ti-6Al-4V alloys, with in situ, synchrotron-based, high-speed, x-ray phase contrast imaging implemented to characterize the dynamic deformation and fracture process of Ti alloys at the Advanced Photon Source. X-ray digital imaging correlation (XDIC) is applied for strain field mapping. The size distribution of x-ray speckles are quantified via a morphological analysis, with a mean of ∼20 μm. Systematic error analyses of displacement and strain field measurements are firstly conducted for XDIC, and demonstrate that the displacement and strain errors can be controlled below 0.01 pixel and 0.1%, respectively. Mesoscale strain characteristics measured via XDIC are consistent with and reveal mechanisms for the bulk-scale stress–strain responses. Under dynamic tension, a sharp transition to strain softening occurs when the bulk strain exceeds about 0.04, which leads to a lower dynamic fracture strain (0.08) than the quasi-static one (0.1). The corresponding strain filed mapping demonstrates that shear deformation localizations grow and coalesce rapidly into a narrow shear deformation band under dynamic loading, while tensile deformation and necking progresses gradually under quasi-static loading. Scanning electron microscopy shows that void nucleation occurs mainly at the interface of α and β phases for both quasi-static and dynamic tension. However, microvoids coalesce preferentially along colony boundaries or the boundary α phase under quasi-static tension, but along the maximum shear stress direction (across colonies) under dynamic tension. Fractography of recovered samples also shows consistent features.

36 MATERIALS SCIENCE↗

Electron microscopy methods in studies of cultural heritage sites

The history of the development and application of scanning electron microscopy (SEM), transmission electron microscopy (TEM), and energy-dispersive X-ray microanalysis (EDXMA) in studies of cultural heritage sites is considered. In fact, investigations based on these methods began when electron microscopes became a commercial product. Currently, these methods, being developed and improved, help solve many historical enigmas. To date, electron microscopy combined with microanalysis makes it possible to investigate any object, from parchment and wooden articles to pigments, tools, and objects of art. Studies by these methods have revealed that some articles were made by ancient masters using ancient “nanotechnologies”; hence, their comprehensive analysis calls for the latest achievements in the corresponding instrumental methods and sample preparation techniques.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Effect of CeLa addition on the microstructures and mechanical properties of Al-Cu-Mn-Mg-Fe alloy

Development of high strength lithium battery shell alloy is highly desired for new energy automobile industry. The microstructures and mechanical properties of Al-Cu-Mn-Mg-Fe alloy with different CeLa additions were investigated through optical microscopy (OM), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Rietveld refinement and tensile testing. Experimental results indicate that Al{sub 8}Cu{sub 4}Ce and Al{sub 6}Cu{sub 6}La phases formed due to CeLa addition. Addition of 0.25 wt.% CeLa could promote the formation of denser precipitation of Al{sub 20}Cu{sub 2}Mn{sub 3} and Al{sub 6}(Mn, Fe) phases, which improved the mechanical properties of the alloy at room temperature. However, up to 0.50 wt.% CeLa addition could promote the formation of coarse Al{sub 8}Cu{sub 4}Ce phase, Al{sub 6}Cu{sub 6}La phase and Al{sub 6}(Mn, Fe) phase, which resulted in weakened mechanical properties. - Highlights: •Al-Cu-Mn-Mg-Fe alloys with different CeLa addition were fabricated through casting and rolling. •Al{sub 8}Cu{sub 4}Ce and Al{sub 6}Cu{sub 6}La phases formed after CeLa addition. •Addition of 0.25 wt.% CeLa promoted formation of denser precipitates of Al{sub 20}Cu{sub 2}Mn{sub 3} and Al{sub 6}(Mn, Fe). •Mechanical properties of the alloy was improved after 0.25 wt.% CeLa addition.

36 MATERIALS SCIENCE↗

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24–500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Influence of Nonstoichiometry on Proton Conductivity in Thin-Film Yttrium-Doped Barium Zirconate

Proton-conducting perovskites have been widely studied because of their potential application as solid electrolytes in intermediate temperature solid oxide fuel cells. Structural and chemical heterogeneities can develop during synthesis, device fabrication, or service, which can profoundly affect proton transport. Here, we use time-resolved Kelvin probe force microscopy, scanning transmission electron microscopy, atom probe tomography, and density functional theory calculations to intentionally introduce Ba-deficient planar and spherical defects and link the resultant atomic structure with proton transport behavior in both stoichiometric and nonstoichiometric epitaxial, yttrium-doped barium zirconate thin films. The defects were intentionally induced through high-temperature annealing treatment, while maintaining the epitaxial single crystalline structure of the films, with an overall relaxation in the atomic structure. As a result, the annealed samples showed smaller magnitudes of local lattice distortions because of the formation of proton polarons, thereby leading to decreased proton-trapping effect. This resulted in a decrease in the activation energy for proton transport, leading to faster proton transport.

36 MATERIALS SCIENCE↗

Isomorphism and solid solutions among Ag- and Au-selenides

Au-Ag selenides were synthesized by heating stoichiometric mixtures of elementary substances of initial compositions Ag{sub 2−x}Au{sub x}Se with a step of x=0.25 (0≤x≤2) to 1050 °C and annealing at 500 °C. Scanning electron microscopy, optical microscopy, electron microprobe analysis and X-ray powder diffraction methods have been applied to study synthesized samples. Results of studies of synthesized products revealed the existence of three solid solutions with limited isomorphism Ag↔Au: naumannite Ag{sub 2}Se – Ag{sub 1.94}Au{sub 0.06}Se, fischesserite Ag{sub 3}AuSe{sub 2} - Ag{sub 3.2}Au{sub 0.8}Se{sub 2} and gold selenide AuSe - Au{sub 0.94}Ag{sub 0.06}Se. Solid solutions and AgAuSe phases were added to the phase diagram of Ag-Au-Se system. Crystal-chemical interpretation of Ag-Au isomorphism in selenides was made on the basis of structural features of fischesserite, naumannite, and AuSe. - Highlights: • Au-Ag selenides were synthesized. • Limited Ag-Au isomorphism in the selenides is affected by structural features. • Some new phases were introduced to the phase diagram Ag-Au-Se.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Thermoelectric properties of Bi{sub 2}Te{sub 2.4}Se{sub 0.6} solid solutions of different particle-size composition

The thermoelectric properties of n-type Bi{sub 2}Te{sub 2.4}Se{sub 0.6} solid solution prepared by the vacuum hot pressing of powder mixtures with different particle sizes are investigated. The powders were prepared by the mechanical grinding of ingots and melt spinning. The microstructure and fracture pattern of a sample cleavage surface are analyzed using scanning electron microscopy and optical microscopy. The thermoelectric characteristics (the Seebeck coefficient, electrical conductivity, and thermal conductivity) are measured at room temperature and in the temperature range of 100–700 K.

36 MATERIALS SCIENCE↗

Physical properties of glasses exposed to Earth-facing and trailing-side environments on LDEF

The exposure of 108 glass samples and 12 glass-ceramic samples to Earth-orbit environments permitted measurements which establish the effects of each environment. Examination of five glass types and one glass ceramic located on both the Earth-facing side and the trailing edge revealed no reduction in strength within experimental limits. Strength measurements subjected less than 5 percent of the sample surface area to stresses above 90 percent of the glass's failure strength. Seven micrometeorite or space debris impacts occurred on trailing edge samples. One of those impacts occurred in a location which was subjected to 50 percent of the applied stress at failure. Micrometeorite or space debris impacts were not observed on Earth-facing samples. The physical shape and structure of the impact sites were carefully examined using stereographic scanning electron microscopy. These impacts induce a stress concentration at the damaged region which influences mechanical strength. The flaw size produced by such damage was examined to determine the magnitude of strength degradation in micrometeorite or space-debris impacted glasses. Scanning electron microscopy revealed topographical details of impact sites which included central melt zones and glass fiber production. The overall crater structure is similar to much larger impacts of large meteorite on the Moon in that the melt crater is surrounded by shocked regions of material which fracture zones and spall areas. Residual stresses arising from shock compression and cooling of the fused zone cannot currently be included in fracture mechanics analyses based on simple flaw size examination.

Wiedlocher, David E.↗

Degradation of Polyester Polyurethane by Aspergillus sp. Strain S45 Isolated from Soil

A polyurethane (PU)-degrading fungus designated as strain S45 was isolated from a solid waste-dumping site in Islamabad, Pakistan. Strain S45 was identified as Aspergillus sp. through microscopic, morphologic as well as 18S rRNA sequencing (99% similarity with Aspergillus fumigatus). The degradation ability of strain S45, was analyzed through measurement of weight loss and evolution of CO{sub 2} as a result of breakdown of PU film. The degradation was confirmed through scanning electron microscopy, fourier transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC). Surface changes like pits, cracks and holes were observed in scanning electron micrographs upon degradation of PU film by strain S45. FTIR spectra were carefully examined, changes were observed in various peaks at different wavelength ranges that also correspond to degradation of PU film. Differential scanning calorimetric technique was used to measure the melting temperature of PU film pieces before and after incubation with strain S45. DSC curve indicated an increase in melting temperature of PU from 191 to 196 °C that might be due to increase in crystallinity of the exposed PU after degradation of amorphous soft segment. A gradual increase in specific activity of esterase was observed up to the maximum of 15th day of incubation with PU film in mineral salt medium. Enzyme activity was further confirmed by tween 20 agar plates, demonstrated by formation of calcium complex. It is concluded from the results that Aspergillus sp. strain S45 might be applied for the treatment of plastics-contaminated environments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Characterisation of organic-inorganic hybrid materials of the types ZnxCd1-xSe(1,3-diaminopropane)1/2 and ZnSySe1-y(1,3-diaminopropane)1/2

Highlights: • New hybrid materials: Zn{sub x}Cd{sub 1-x}Se(1,3-DAP){sub 1/2} and ZnS{sub x}Se{sub 1-x}(1,3-DAP){sub 1/2} were obtained. • Hybrids were studied using XRD, TG/DSC, XRD vs. temperature, SEM, UV–vis spectroscopy. • The impact of the composition of the layers on optical properties were studied. - Abstract: Organic-inorganic hybrid materials of the type MeQ(diamine){sub 1/2} (where Me–Zn, Cd, Mn and Q–S, Se, Te) belong to the class of 3D nanomaterials. They are built of layers of II–VI semiconductors and amines, which act as linkers. The main goal of our work was the synthesis of compounds of the type Zn{sub x}Cd{sub 1-x}Se(1,3-diaminopropane){sub 1/2} and ZnS{sub y}Se{sub 1-y}(1,3-diaminopropane){sub 1/2} (where x, y = 0, 0.25, 0.5, 0.75, 1) and the study of properties changed by the composition of the semiconducting layers. Analysis of these materials was carried out with the use of X-ray powder diffraction (XRPD), scanning electron microscopy (SEM), simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC) as well as temperature dependent XRPD enabled us to obtain information about the thermal stability of hybrid compounds with mixed semiconducting layers. Another important part of our work was a study, performed with the use of UV–vis spectroscopy, of the optical properties of these materials.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Random anion distribution in MS x Se 2- x (M = Mo, W) crystals and nanosheets

The group VIb dichalcogenides (MX 2 , M = Mo, W; X= S, Se) have a layered molybdenite structure in which M atoms are coordinated by a trigonal prism of X atoms. Ternary solid solutions of MS x Se 2– x were synthesized, microcrystals were grown by chemical vapor transport, and their morphologies and structures were characterized by using synchrotron X-ray diffraction, Rietveld refinement, DIFFaX simulation of structural disorder, scanning electron microscopy, and energy dispersive X-ray spectroscopy. Double aberration corrected scanning transmission electron microscopy was used to determine the anion distributions in single-layer nanosheets exfoliated from the microcrystals. These experiments indicate that the size difference between S and Se atoms does not result in phase separation, consistent with earlier studies of MX 2 monolayer sheets grown by chemical vapor deposition. However, stacking faults occur in microcrystals along the layering axis, particularly in sulfur-rich compositions of MS x Se 2– x solid solutions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Utah FORGE: Well 16A(78)-32 Core Analysis Results

This dataset features petrographic, X-Ray Diffraction (XRD), and Scanning Electron Microscopy Analyses of core samples from well 16A(78)-32, which serves as the injection well for the Utah FORGE Enhanced Geothermal System (EGS) project. In addition to an overview of the analysis, the following items have been included here: images of 21 entire thin sections in plane-polarized and cross-polarized light from 16 depths, scanning electron microscope back scatter electron photomosaic maps of 21 thin sections from 16 depths, bulk XRD data from 16 depths, clay-sized XRD patterns from 16 depths, an optical petrography report, and scanning electron microscopy and energy dispersive spectroscopy analyses of eight selected samples.

15 GEOTHERMAL ENERGY↗

Study of phase transformation and microstructure of alcohol washed titania nanoparticles for thermal stability

Nanostructured titania have been successfully synthesized by hydrolysis of alkoxide at calcination temperatures 500 °C, 600 °C and 700 °C. As the calcination temperature increases, alcohol washed samples show lesser rutile content as compared to water washed samples. Morphology and Particle sizes was determined by field emission scanning electron microscopy (FESEM), while thermogravimetric-differential scanning calorimetry (TG-DSC) was used to determine thermal stability. Alcohol washed samples undergo 30% weight loss whereas 16% in water washed samples was observed. The mean particle sizes were found to be increase from 37 nm to 100.9 nm and 35.3 nm to 55.2 nm for water and alcohol washed samples respectively. Hydrolysis of alkoxide was shown to be an effective means to prepare thermally stable titania by using alcohol washed samples as a precursor.

36 MATERIALS SCIENCE↗

Emerging hierarchical dislocation structures: Insights from scanning electron microscopy-electron backscatter diffraction in situ tensile testing and multifractal analysis

Understanding the evolution of dislocation structures during plastic deformation is critical for predicting the mechanical performance of metallic materials. In this work, we applied in situ scanning electron microscopy/electron backscatter diffraction tensile testing combined with multifractal (MF) analysis to assess deformation-induced dislocation structure evolution in solution-annealed 304 L stainless steel, both in its as-received and neutron-irradiated states (5.4 displacements per atom). The analysis of kernel average misorientation patterns revealed the formation of hierarchical dislocation arrangements that exhibit clear MF scaling behavior. Despite pronounced visual differences between nonirradiated and irradiated specimens—most notably, the appearance of dislocation channels after irradiation—the singularity spectra suggest that both conditions give rise to similar underlying hierarchical structures. MF analysis provides a quantitative measure of the spatial complexity and self-organization of dislocation patterns, highlighting the accelerated emergence and evolution of the dislocation structures in irradiated polycrystalline materials, as well as the limitation of their spatial extent. The findings indicate that irradiation not only modifies microstructure but also alters correlation-driven dislocation organization. More generally, they demonstrate that MF analysis is a powerful tool for probing mesoscale deformation mechanisms.

Dislocation structures↗

Interaction Between Liquid Silver and Graphene-Coated SiC Substrate

Wettability between liquid Ag and graphene-coated SiC single crystal has been investigated by dispensed drop method at T = 970 °C under vacuum accompanied with subsecond recording of the drop/substrate images (100 frames per second) by high-speed high-resolution CCD camera. Non-contact heating method coupled with capillary purification of the Ag drop procedure has been applied. Scanning electron microscopy combined with EDS analysis and scanning probe microscopy combined with Raman spectroscopy techniques has been utilized for microstructure and surface characterization of samples before and after high-temperature wetting tests. Immediately after its detachment from the capillary, the Ag drop showed non-wetting behavior (θ > 90°) forming a high contact angle of θ = 114°. Surface characterization of the drop surface after wettability tests evidenced the presence of graphene and Si transferred from the substrate to the top of Ag drop. These findings suggest chemical interaction phenomena occurring at the interface. Locally, an intimate contact between liquid Ag and SiC substrate was allowed by the appearance of discontinuities in the graphene layer basically produced by thermomechanical stress. Local dissolution of carbon into liquid Ag and its reorganization (by segregation, nucleation and growth) as secondary graphene layer at the Ag surface was also observed.

36 MATERIALS SCIENCE↗

Nanosized low-temperature phases of titanium(IV) oxide with anatase and η-phase structures: composition, structure, and photocatalytic properties

Nanosized low-temperature modifications of titanium(IV) oxide with the anatase and η-phase (TiO{sub 2–x}•mH{sub 2}O) structures were prepared by the sulfate method (pH <3) and for the first time characterized by a complex of methods (X-ray diffractometry, scanning electron microscopy, IR spectroscopy, Raman spectroscopy, differential scanning calorimetry, low-temperature sorption capacity of samples to nitrogen, and differentiating dissolution). The physicochemical properties of the modifications were compared. Differences in compositions of the surface and volumes of the samples, compositions and structures of the phases (structure of η-phase is superstructure to anatase), and microstructure elements (sizes of crystallites, nanoparticles, and specific surface area; volume of nano- and ultrananopores) were revealed. The region of η-phase stability was found in the coordinates of temperature (T = 50–95 °C) and hydrolysis duration (τ = 10–80 min) and temperature (T≤200 °C) and annealing duration (τ <6 h). The distinctions in the thermal behavior of the nanosized anatase and η-phase were studied. The photocatalytic activity (PCA) is determined by the physicochemical characteristics of the samples and phases and also by the composition and structure of the decomposed substrate. In the case of difenoxazole, the PCA is affected by the compositions of the samples, phases, and surface (the presence of OH groups) and specific surface area, whereas the composition of the samples and specific surface area affect the PCA in the case of thiamethoxam.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Effect of annealing on Curie temperature and phase transition in La{sub 0.55}Sr{sub 0.08}Mn{sub 0.37}O{sub 3} epitaxial films grown on SrTiO{sub 3} (100) substrates by reactive radio frequency magnetron sputtering

Mn-poor LaSrMnO{sub 3} (LSMO) epitaxial films were grown on SrTiO{sub 3} (100) substrates by radio frequency magnetron sputtering in an argon and oxygen gas mix, and then the samples were annealed in air at various temperatures (T{sub a}). 2 theta-chi X-ray diffraction mapping, nano-beam diffraction analysis through transmission electron microscopy, and electron back scatter diffraction through scanning electron microscopy revealed that the crystal symmetry of the LSMO films changed from monoclinic/orthorhombic to rhombohedral on annealing in air. Curie temperature (T{sub C}) of the LSMO films was found to increase with increasing T{sub a}, and become higher than the room temperature at T{sub a} ≥ 861 °C, indicating that the cause of these changes was the filling of oxygen and the transition of the crystal symmetry into rhombohedral. - Highlights: •Mn-poor LSMO changed from monoclinic/orthorhombic to rhombohedral by oxygen supply. •Mn-poor LSMO was increased T{sub C} by changed crystal symmetry, and it showed T{sub C} above RT. •Annealed in air effectively supplied O{sub 2} more than O{sub 2} gas during sputtering •EBSD is useful to evaluate crystal symmetry of complex oxide film from the substrate.

36 MATERIALS SCIENCE↗