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At least 181 records · Page 10

Large grain CBMM Nb ingot slices: An ideal test bed for exploring the microstructure-electromagnetic property relationships relevant to SRF

High purity (RRR > 200), large grain (> 5-10 cm) niobium ingot slices have been successfully used to fabricate radio frequency (RF) cavities for particle accelerators. They offer significantly reduced fabrication cost by eliminating processing steps and furthermore they provide the opportunity to study the influence of individual grain boundaries in SRF Nb. Here we summarize our measurements of grain boundary (GB) effects on the superconducting properties of large grain high purity niobium sheet manufactured by CBMM. We show by magneto-optical (MO) imaging that GBs allow premature flux penetration, but only when they are oriented close to the direction of the magnetic field. However, even low angle GBs produced by minor deformations commensurate with half-cell forming produce localized flux penetration. The transport properties of grain boundaries were investigated by direct transport across them and evidence for preferential vortex flow along the GBs of SRF Nb was observed for the first time. Using transmission electron microscopy (TEM) and micro crystallographic analysis with electron backscattered diffraction (EBSD), we were able to quantitatively characterize surface substructures that can lead to localized thermal breakdown of superconductivity. Important to these studies was the development of sample preparation techniques that made the cutout single, bi-crystal and tri-crystal Nb coupons as representative as possible of the surface properties of cavities manufactured by standard techniques.

36 MATERIALS SCIENCE↗

Beam current effect as a potential challenge in SEM-EBSD in situ tensile testing

Highlights: • In situ SEM-EBSD tensile tests were conducted using 304L steels with 8 and 10.4% Ni. • KAM and GROD evolution, twinning, and phase instability were investigated. • Phase transformation in 8% Ni-steel was sensitive to the electron beam current. In situ mechanical tensile tests coupled with electron backscatter diffraction (EBSD) analysis were conducted using specimens of two 304L steels with ~8 and 10.4% Ni content, respectively. Twinning was observed in steel with 10.4% Ni content, whereas steel with 8% Ni content demonstrated martensitic transformation. Testing showed that the kinetics of martensitic transformation in steel with 8% Ni content was influenced by the electron beam current used during EBSD scans. Continuous scanning using 32 nA nominal beam current led to suppression of the phase instability in the near-surface layer, but acceptable comparable-to-the-bulk results were obtained using 8 nA beam current. The exact mechanism of the beam current role is unclear, but it appears to be neutral regarding Kernel Average Misorientation behavior and deformation-induced twinning.

36 MATERIALS SCIENCE↗

Physical and electrical properties of melt-spun Fe-Si (3–8 wt.%) soft magnetic ribbons

Highlights: • Increasing processing wheel speed during melt spinning refined both the ribbon cross-sectional thickness and grain size. • Mössbauer studies indicated Si content influenced the number of Fe sites and the magnetic field/structural environments. • Vickers hardness and the elastic modulus were observed to increase in response to elevated Si content and wheel speed. • Increasing Si content diluted the magnetization. - Abstract: Fe-Si alloys ranging from 3 to 8 wt% Si were rapidly solidified using melt spinning. Wheel speeds of 30 m/s and 40 m/s were employed to vary cooling rates. Mössbauer spectroscopic studies indicated the Si content significantly influenced the number of Fe sites, relative abundance of various Fe species, and internal magnetic fields/structural environments. Wheel speed altered Fe speciation only in the 3 wt% sample. Scanning electron microscopy confirmed that increasing the wheel speed refined both the ribbon thickness and grain size. Electron backscatter diffraction results suggest tailoring melt spinning process parameters and alloy chemistry may offer the ability to manipulate {001} texture development. Electrical resistivity measurements were observed to increase in response to elevated Si content. Increased hardness was correlated to elevated Si content and wheel speed.

36 MATERIALS SCIENCE↗

Enhanced thermoelectric performance in spark plasma textured bulk n-type BiTe{sub 2.7}Se{sub 0.3} and p-type Bi{sub 0.5}Sb{sub 1.5}Te{sub 3}

Bulk p and n-type bismuth tellurides were prepared using spark plasma texturization method. The texture development along the uniaxial load in the 001 direction is confirmed from both x-ray diffraction analysis and electron backscattering diffraction measurements. Interestingly, those textured samples outperform the samples prepared by conventional spark plasma sintering (SPS) leading to a reduced thermal conductivity in the ab-plane. The textured samples of n-type BiTe{sub 2.7}Se{sub 0.3} and p-type Bi{sub 0.5}Sb{sub 1.5}Te{sub 3} showed a 42% and 33% enhancement in figure of merit at room temperature, respectively, as compared to their SPS counterparts, opening the route for applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

In situ synchrotron X-ray diffraction analysis of ultrasonically assisted microstructure refinement during laser melting process

This work investigates the effect of ultrasonic treatment (UST) on the microstructure of AA4043 alloy during laser melting process. Here, the study utilizes in situ synchrotron X-ray diffraction (SXRD) and postmortem electron backscatter diffraction (EBSD) techniques to examine the ultrasonic grain refinement mechanism. The SXRD diffraction patterns exhibit higher continuity of major diffraction rings in the UST-test pattern, indicating a more refined grain structure. The presence of new diffraction spots in the post-test diffraction pattern with UST suggests the breakdown of epitaxial growth of columnar dendrites during solidification. Thermal profiles determined by analyzing the lattice parameter evolution show a faster cooling rate with UST. The inverse pole figures and aspect ratio distribution from EBSD reveal that the UST samples exhibit a refined, more equiaxed grain structure along the weld centerline. UST sample also develops more fine-sized low angle grain boundaries (LAGBs). These features offer better hot-cracking resistance in aluminum alloys.

36 MATERIALS SCIENCE↗

A novel ultrafine-grained Fe−22Mn−0.6C TWIP steel with superior strength and ductility

A fully recrystallized ultrafine-grained (UFG) Fe−22wt.%Mn−0.6wt.%C twinning-induced plasticity (TWIP) steel with mean grain size of 576 nm was fabricated by cold rolling and annealing process. Tensile test showed that this UFG steel possessed high yield strength of 785 MPa, and unprecedented uniform elongation of 48%. The Hall-Petch relationship was verified from the coarse-grained (CG) regime to the ultrafine-grained (UFG) regime. The microstructures at specified tensile strains were characterized by electron backscattered diffraction (EBSD) and transmission electron microscopy (TEM). The microstructures and strain hardening behavior of the UFG TWIP steel were compared with the CG counterpart. The strong strain hardening capability of the UFG steel is supposed to be responsible for the high strength and good ductility. - Highlights: • A fully recrystallized Fe−22Mn−0.6C TWIP steel with mean grain size of 576 nm was fabricated. • The ultrafine-grained (UFG) steel exhibits strong strain-hardening capability, excellent strength and ductility. • The Hall-Petch relationship is fitted well from the CG regime to the UFG regime.

36 MATERIALS SCIENCE↗

Characterization of multilayer nitride coatings by electron microscopy and modulus mapping

This paper discusses multi-scale characterization of physical vapour deposited multilayer nitride coatings using a combination of electron microscopy and modulus mapping. Multilayer coatings with a triple layer structure based on TiAlN and nanocomposite nitrides with a nano-multilayered architecture were deposited by Cathodic arc deposition and detailed microstructural studies were carried out employing Energy Dispersive Spectroscopy, Electron Backscattered Diffraction, Focused Ion Beam and Cross sectional Transmission Electron Microscopy in order to identify the different phases and to study microstructural features of the various layers formed as a result of the deposition process. Modulus mapping was also performed to study the effect of varying composition on the moduli of the nano-multilayers within the triple layer coating by using a Scanning Probe Microscopy based technique. To the best of our knowledge, this is the first attempt on modulus mapping of cathodic arc deposited nitride multilayer coatings. This work demonstrates the application of Scanning Probe Microscopy based modulus mapping and electron microscopy for the study of coating properties and their relation to composition and microstructure. - Highlights: • Microstructure of a triple layer nitride coating studied at multiple length scales. • Phases identified by EDS, EBSD and SAED (TEM). • Nanolayered, nanocomposite structure of the coating studied using FIB and TEM. • Modulus mapping identified moduli variation even in a nani-multilayer architecture.

36 MATERIALS SCIENCE↗

Microstructure and texture evolution of Cu–Nb composite wires

The evolution of microstructure and texture in Cu–Nb composite wires fabricated by an accumulative drawing and bundling process was investigated by backscattered electron (BSE), electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM). Results indicate the onset of severe curling and shape changing occurred at the size of Nb ∼ 400 nm with a surface increase of about 6.91 μm{sup 2}/μm{sup 3} (the area per unit volume). Two kinds of grain boundaries in Nb are suggested: one is 20°–50° boundary with a rotate/tilt axis around <110> parallel to drawing direction (DD), and another is > 50° boundary with the axis perpendicular to DD. The curling phenomenon occurred at the Cu–Nb interface and is related not only to the deformation mechanism of Nb but also to the presence of interface. This result is distinct from reported works showing that curling takes place when BCC metals are heavily drawn (Area reduction > 73%). The variation in microstructure and texture evolution between Cu and Nb filaments was discussed based on the differences in deformation mechanisms of these two metals. - Highlights: • Microstructure and texture evolution were studied systematically by EBSD. • In Nb, grain boundaries of 20°–50° have a rotate/tile axis around <110>//DD. • The rotation axes of above 50° boundaries are concentrated around <111> ⊥ DD in Nb. • Curling is related to not only deformation mode of BCC but also Cu–Nb interface.

36 MATERIALS SCIENCE↗

High- and Low-Temperature Deformation Behavior of Different Orientation Hot-Rolled Annealed Zircaloy-4

In this paper, the hot-rolled annealed Zircaloy-4 samples with different orientation were subjected to uniaxial compression with a strain rate of 0.001 s{sup −1} to obtain the stress-strain curves of different initial orientation samples at different temperatures. Electron backscatter diffraction (EBSD) technique and transmission electron microscope (TEM) technique were used to analyze the microstructures and textures of compressed samples. The mechanical properties and microstructural evolution of rolling directions (RD), transverse directions (TD) and normal directions (ND) were investigated under the conditions of – 150 °C low temperature, room temperature and 200 °C high temperature (simulated lunar temperature environment). The results show that the strength of Zircaloy-4 decreases with the increase in deformation temperature, and the strength in three orientations is ND > TD > RD. The deformation mechanism of hot-rolled annealed Zircaloy-4 with different orientation is different. In RD, {101̄0}〈a〉 prismatic slip has the highest Schmid factor (SF), so it is most easy to activate the slip, followed by TD orientation, and ND orientation is the most difficult to activate. The deformed grains abide slip→twinning→slip rule, and the different orientation Zircaloy-4 deformation mechanisms mainly are the twinning coordinated with the slip.

36 MATERIALS SCIENCE↗

Hardness and modulus of Fe2B, Fe3(C,B), and Fe23(C,B)6 borides and carboborides in the Fe-C-B system

Highlights: • Hardness and modulus of the Fe{sub 2}B, Fe{sub 3}(C,B), Fe{sub 23}(C,B){sub 6} and M{sub 7}C{sub 3} phases are analyzed. • Hardness and modulus of the Fe{sub 3}(C,B) phase are increasing with its B content. • Size effects are apparent for hardness of Fe{sub 2}B, Fe{sub 3}(C,B), Fe{sub 23}(C,B){sub 6} and M{sub 7}C{sub 3}. • The model of Nix and Gao was used to evaluate the load-independent hardness H{sub 0}. • Hardness ranking is Fe{sub 2}B > M{sub 7}C{sub 3} > Fe{sub 3}(C,B) > Fe{sub 23}(C,B){sub 6} - Abstract: This work provides a comparative and comprehensive study of the indentation hardness and indentation modulus of iron-rich borides and carboborides of types Fe{sub 2}B, Fe{sub 3}(C,B), and Fe{sub 23}(C,B){sub 6}. In addition, the hardness and elastic modulus of Cr-rich M{sub 7}C are investigated for comparative purposes. We investigated the impact of increasing B content and indentation size effect (ISE). The phases of interest were stabilized in cast Fe-C-B alloys that varied with respect to the B / (B + C) ratio and heat treatment. The resulting microstructures were characterized by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), electron backscatter diffraction (EBSD), and wavelength X-ray spectroscopy (WDS). Dynamic in-situ nanoindentation experiments based on the method of continuous stiffness measurement (CSM) were coupled to SEM and EBSD investigations to determine the mechanical properties of the individual borides and carboborides as a function of the indentation depth. The results were compared to values obtained for the Cr-rich M{sub 7}C{sub 3} carbide. It was found that the hardness of the B-rich Fe{sub 3}(C{sub ,}B) phase is considerably higher than pure Fe{sub 3}C and increases with increasing B content. The ISE was present in all investigated phases, and the hardness decreased as a function of indentation depth. The hardness at infinite indentation depth H{sub 0} was estimated according to the model of Nix and Gao. The Fe{sub 2}B phase was found to be the hardest phase (H{sub 0} = 19.04 GPa), followed by M{sub 7}C{sub 3} (H{sub 0} = 16.43 GPa), Fe{sub 3}(C,B) (H{sub 0} = 11.18 to 12.24 GPa), and Fe{sub 23}(C,B){sub 6} (H{sub 0} = 10.39 GPa).

36 MATERIALS SCIENCE↗

Effect of heat input on the microstructure, residual stresses and corrosion resistance of 304L austenitic stainless steel weldments

Austenitic stainless steels are widely used in high performance pressure vessels, nuclear, chemical, process and medical industry due to their very good corrosion resistance and superior mechanical properties. However, austenitic stainless steels are prone to sensitization when subjected to higher temperatures (673 K to 1173 K) during the manufacturing process (e.g. welding) and/or certain applications (e.g. pressure vessels). During sensitization, chromium in the matrix precipitates out as carbides and intermetallic compounds (sigma, chi and Laves phases) decreasing the corrosion resistance and mechanical properties. In the present investigation, 304L austenitic stainless steel was subjected to different heat inputs by shielded metal arc welding process using a standard 308L electrode. The microstructural developments were characterized by using optical microscopy and electron backscattered diffraction, while the residual stresses were measured by X-ray diffraction using the sin{sup 2}ψ method. It was observed that even at the highest heat input, shielded metal arc welding process does not result in significant precipitation of carbides or intermetallic phases. The ferrite content and grain size increased with increase in heat input. The grain size variation in the fusion zone/heat affected zone was not effectively captured by optical microscopy. This study shows that electron backscattered diffraction is necessary to bring out changes in the grain size quantitatively in the fusion zone/heat affected zone as it can consider twin boundaries as a part of grain in the calculation of grain size. The residual stresses were compressive in nature for the lowest heat input, while they were tensile at the highest heat input near the weld bead. The significant feature of the welded region and the base metal was the presence of a very strong texture. The texture in the heat affected zone was almost random. - Highlights: • Effect of heat input on microstructure, residual stresses and corrosion is studied. • HAZ and width of dendrite in the welded region increase with heat input. • Residual stresses are tensile near the welded region after the highest heat input. • Welded region has the highest pit density after highest heat input. • Dendrites and δ-ferrite were highly oriented in the welded region.

36 MATERIALS SCIENCE↗

Martensitic Transformation in Fe x Mn 80-x Co 10 Cr 10 High-Entropy Alloy

High-entropy alloys and even medium-entropy alloys are an intriguing class of materials in that structure and property relations can be controlled via alloying and chemical disorder over wide ranges in the composition space. Employing density-functional theory combined with the coherent-potential approximation to average over all chemical configurations, we tune free energies between face-centered-cubic and hexagonal-close-packed phases in Fe x Mn 80 - x Co 10 Cr 10 systems. Within Fe-Mn-based alloys, we show that the martensitic transformation and chemical short-range order directly correlate with the face-centered-cubic and hexagonal-close-packed energy difference and stacking-fault energies, which are in quantitative agreement with recent observation of two phase region (face-centered cubic and hexagonal closed pack) in a polycrystalline high-entropy alloy sample at x = 40 at.%. Our predictions are further confirmed by single-crystal measurements on a x = 40 at.% using transmission-electron microscopy, selective-area diffraction, and electron-backscattered-diffraction mapping. The results herein offer an understanding of transformation-induced or twinning-induced plasticity in this class of high-entropy alloys and a design guide for controlling the physics at the electronic level.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Interrupted in situ EBSD study of texture evolution and mechanism of surface grains in electroformed Ni after annealing with an initially duplex <100> + <111> fiber texture during uniaxial tensile deformation

Highlights: • The texture evolution of the electroformed Ni was investigated by using an interrupted in situ electron backscattered diffraction. • The initial <100> fiber component evolved into the metastable cube component with a weaker copper component. • Only a few grains of the initial <111> fiber component evolved into the copper orientation. - Abstract: The texture evolution process and mechanism of surface grains in electroformed Ni after annealing with an initially duplex <100> + <111> fiber texture during uniaxial tensile deformation were investigated by using interrupted in situ electron backscattered diffraction. The results showed that the initially duplex <100> + <111> fiber texture evolved into the metastable Cube orientation with a weak Cu orientation during the uniaxial tensile deformation. The volume fractions of <100> and <111> fiber texture decreased from 54.0% to 29.3% and 16.6% to 6.6%, respectively. The volume of the Cube orientation remained almost stable at 12%, whereas that of the Cu orientation increased from 1% to 2.9%. A simulation of the final preferred orientation based on the Taylor model was a cubic texture, which qualitatively agreed well with the experimental result. The simulated results indicated that the formed Cube and Cu textures evolved from the initial <100> and <111> fiber textures, respectively.

36 MATERIALS SCIENCE↗

Crystallographic Texture and Orientation Variants in Al2O3-Y3Al5O12 Directionally Solidified Eutectic Crystals

Eutectic rods of Al2O3 and Y3Al5O12 were grown by a laser-heated float zone method, and their microstructure and crystallographic texture were studied by scanning electron microscopy, electron backscattered diffraction and x-ray diffraction. The composites were found to be highly textured with two twin-related crystallographic orientation relationships between the phases. Electron backscattered diffraction was employed to determine the spatial distribution of the orientational variants within the samples and to define the crystallographic orientation of various microstructural features.

Frazer, Colleen S.↗

Influence of current density on microstructure of pulse electrodeposited tin coatings

Pulse electrodeposited tin coatings on copper substrate have been synthesized from an aqueous solution containing sodium stannate (Na{sub 2}SnO{sub 3}.3H{sub 2}O) and sodium hydroxide (NaOH). The effect of current density on surface morphology of the deposits has been investigated. As deposited coatings are characterized by X-ray diffraction, scanning electron microscopy, electron backscatter diffraction, and line profile analysis. The X-ray diffraction analysis shows that the deposits consist of tetragonal ({beta}-Sn) structure with microcrystalline grains. The deposits plated at lower current density exhibit (110) texture which decreases with increasing current densities. The effects of current density on Cu-Sn diffusion and whisker growth of the electrodeposited tin coatings are also reported here. - Highlights: Black-Right-Pointing-Pointer Pulse electrodeposition of Sn from aqueous alkaline solution without adding any organic additive. Black-Right-Pointing-Pointer Effect of current density on morphology and whisker growth in tin coatings aged for 1 year. Black-Right-Pointing-Pointer Solution bath is stable and can be operated over a wide range of current density.

36 MATERIALS SCIENCE↗

Characterizing defect structures in AM steel using direct electron detection EBSD

The mechanical properties of additive and traditionally manufactured alloys are largely dependent on the characteristics and distribution of dislocation cell networks that develop during the fabrication process. This work demonstrates the ability to quantitatively characterize these dislocation structures by high angular resolution electron backscatter diffraction analysis using a direct electron detector. The defect structures are characterized in terms of the geometrically necessary dislocation density and the associated Burgers vector and line direction. Furthermore, the results are discussed in terms of potential defect formation mechanisms.

36 MATERIALS SCIENCE↗

High-cycle fatigue behavior of Ti-5Al-2.5Sn ELI alloy forging at low temperatures

High-cycle fatigue properties of Ti-5Al-2.5Sn Extra Low Interstitial (ELI) alloy forging were investigated at low temperatures. The high-cycle fatigue strength at low temperatures of this alloy was relatively low compared with that at ambient temperature. The crystallographic orientation of a facet formed at a fatigue crack initiation site was determined by electron backscatter diffraction (EBSD) method in scanning electron microscope (SEM) to understand the fatigue crack initiation mechanism and discuss on the low fatigue strength at low temperature. Furthermore, in terms of the practical use of this alloy, the effect of the stress ratio (or mean stress) on the high-cycle fatigue properties was evaluated using the modified Goodman diagram.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Assessing Manufacturability of the Oxide Dispersion Strengthened (ODS) 14YWT Alloy Fuel Cladding Tube Using SolidStir™ Technology

The 14YWT (Fe–14Cr–3W–0.4Ti–0.3Y2O3 (wt.%)) alloy is a potential candidatematerial for fabricating fuel cladding tubes and other structural components to be used in next-generation advanced nuclear reactors. Due to inherent limitations of current processing routes, this research explored a new variant of friction stir processing, commercially referred to as SolidStir™ Extrusion (patent pending) technology from Enabled Engineering to consolidate and extrude 14YWT powder into a fuel cladding tube. Several single-layer and multiple-layer consolidation experiments were carried out in an Inconel 625 die to determine the suitable processing parameters for SolidStir™ extrusion of the 14YWT alloy cladding tube. With these processing parameters, a 16–18 mm long tube of the 14YWT alloy with no visible defects was successfully extruded using this novel technology. Microstructural characterization results obtained using optical microscopy, scanning electron microscopy, energy dispersive spectroscopy, electron backscatter diffraction, and transmission electron microscopy will be presented.

Advanced Materials and Manufacturing Technology↗