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At least 1,117 records · Page 62

Using defects as a ‘fossil record’ to help interpret complex processes during additive manufacturing: as applied to raster-scanned electron beam powder bed additively manufactured Ti–6Al–4V

Abstract Defects in parts produced by additive manufacturing, instead of simply being perceived as deleterious, can act as important sources of information associated with the complex physical processes that occur during materials deposition and subsequent thermal cycles. Indeed, they act as materials-state ‘fossil’ records of the dynamic AM process. The approach of using defects as epoch-like records of prior history has been developed while studying additively manufactured Ti–6Al–4V and has given new insights into processes that may otherwise remain either obscured or unquantified. Analogous to ‘epochs,’ the evolution of these defects often is characterized by physics that span across a temporal length scale. To demonstrate this approach, a broad range of analyses including optical and electron microscopy, X-ray computed tomography, energy-dispersive spectroscopy, and electron backscatter diffraction have been used to characterize a raster-scanned electron beam Ti–6Al–4V sample. These analysis techniques provide key characteristics of defects such as their morphology, location within the part, complex compositional fields interacting with the defects, and structures on the free surfaces of defects. Observed defects have been classified as banding, spherical porosity, and lack of fusion. Banding is directly related to preferential evaporation of Al, which has an influence on mechanical properties. Lack-of-fusion defects can be used to understand columnar grain growth, fluid flow of melt pools, humping, and spattering events. Graphical abstract

36 MATERIALS SCIENCE↗

Us army corps of engineers - Engineering research and development center - Petrographic analysis of section 3 personnel tunnel concrete

The Concrete and Materials Branch (CMB) of the Geotechnical and Structures Laboratory was requested to perform an analysis on concrete cores collected from the north and south walls of the H-Canyon Section 3 Personnel Tunel, Savannah River Site, Aiken, South Carolina to determine the cause of the lower than expected compressive strength. This study examined five cores provided to the ERDC by the Department of Energy. The cores were logged in as CMB No. 170051-1 to 170051-5 and subjected to petrographic examination, air void analysis, chemical sprays, scanning electron microscopy, and x-ray diffraction.

##CAI suggestions##↗

Correlation of Processing and Structure in an Ethylene‐Glycol Side‐Chain Modified Polythiophene via Combined X‐Ray Scattering and 4D Scanning Transmission Electron Microscopy

The results of a combined grazing incidence wide-angle X-ray scattering (GIWAXS) and 4D scanning transmission microscopy (4D-STEM) analysis of the effects of thermal processing on poly(3[2-(2-methoxyethoxy)ethoxy]-methylthiophene-2,5-diyl) are reported, a conjugated semiconducting polymer used as the active layer in organic electrochemical transistor devices. GIWAXS provides a measure of overall crystallinity in the film, while 4D-STEM produces real-space maps of the morphology and orientation of individual crystallites along with their spatial extent and distribution. The sensitivity of the 4D-STEM detector allows for collection of electron diffraction patterns at each position in an image scan while limiting the imparted electron dose to below the damage threshold. In conclusion, the effects of heat treatment on the distribution and type of crystallites present in the films is determined.

36 MATERIALS SCIENCE↗

B2 Grain Growth Behavior of a Ti-22Al-25Nb Alloy Fabricated by Hot Pressing Sintering

Grain growth behavior of a powder metallurgy (P/M) Ti-22Al-25Nb alloy was investigated by applying a series of isothermal treatment tests over a wide range of temperatures and holding times. An isothermal treatment scheme was conducted in the B2 phase region (1070-1110 °C) and α{sub 2} + B2 phase region (1010-1050 °C) at holding times of 10, 30 min, 1, 2, and 3 h, respectively. The effects of temperature and holding time on the microstructure evolution and microhardness of the P/M Ti-22Al-25Nb alloy at elevated temperatures were evaluated using optical microscope, scanning electron microscope, x-ray diffraction, and Vickers hardness test techniques. The results revealed that the alloy’s treated microstructure was closely linked to temperature and holding time, respectively. The change law of B2 grain growth with holding time and temperature can be well interpreted by the Beck equation and Hillert equation, respectively. The B2 grain growth exponent n and activation energy Q were acquired based on experimental data in the α{sub 2} + B2 and B2 phase regions. In addition, the grain growth contour map for the P/M Ti-22Al-25Nb alloy was constructed to depict variations in B2 grain size based on holding time and temperature.

36 MATERIALS SCIENCE↗

High quality transmission Kikuchi diffraction analysis of deformed alloys - Case study

Modern scanning electron microscopes (SEM) equipped with thermally assisted field emission guns (Schottky FEG) are capable of imaging with a resolution in the range of several nanometers or better. Simultaneously, the high electron beam current can be used, which enables fast chemical and crystallographic analysis with a higher resolution than is normally offered by SEM with a tungsten cathode. The current resolution that limits the EDS and EBSD analysis is related to materials' physics, particularly to the electron-specimen interaction volume. The application of thin, electron-transparent specimens, instead of bulk samples, improves the resolution and allows for the detailed analysis of very fine microstructural features. Beside the typical imaging mode, it is possible to use a standard EBSD camera in such a configuration that only transmitted and scattered electrons are detected. This modern approach was successfully applied to various materials giving rise to significant resolution improvement, especially for the light element magnesium based alloys. This paper presents an insight into the application of the transmission Kikuchi diffraction (TKD) technique applied to the most troublesome, heavily-deformed materials. In particular, the values of the highest possible acquisition rates for high resolution and high quality mapping were estimated within typical imaging conditions of stainless steel and magnesium-yttrium alloy. - Highlights: •Monte Carlo simulations were used to simulate EBSD camera intensity for various measuring conditions. •Transmission Kikuchi diffraction parameters were evaluated for highly deformed, light and heavy elements based alloys. •High quality maps with 20 nm spatial resolution were acquired for Mg and Fe based alloys. •High speed TKD measurements were performed at acquisition rates comparable to the reflection EBSD.

36 MATERIALS SCIENCE↗

Preliminary Examination of Returned Samples From Bennu Using Quantitative Particle Analysis in the Scanning Electron Microscope

The sample of regolith collected from asteroid Bennu by NASA’s OSIRIS-REx spacecraft will land in Utah on September 24, 2023. A 100-mg aliquot of fine Bennu dust adhering to the internal surfaces of the sample return capsule and associated hardware will be collected by curation staff during disassembly and analyzed immediately by members of the sample analysis team in a “Quick-Look” (Q-L) procedure. The Q-L objectives are (1) to provide images for release to the public to inform on the nature of the returned sample, and (2) to perform a reconnaissance investigation of the mineralogic characteristics of the returned material for science purposes. We will determine the minerals that occur in the dust, assess their diversity, and determine relative abundances at the >5% level using a combination of optical microscopy, Fourier-transform infrared spectroscopy, X-ray powder diffraction, and field-emission scanning electron microscopy (SEM). Here we describe the procedures and techniques developed for the Q-L analyses using analog samples analyzed by SEM equipped with energy dispersive X-ray spectroscopy (EDX). To test these techniques, we have applied them to several samples, including powders of the Murchison (Fig. 1) and Orgueil meteorites, as well as simulant samples prepared by the mission.

OSIRIS-REx↗

Laser Fabrication of Two-Dimensional Rotating-Lattice Single Crystal

A rotating lattice single (RLS) crystal is a unique form of solid, which was fabricated recently as one-dimensional architecture in glass via solid state transformation induced by laser irradiation. In these objects, the lattice rotates gradually and predictably about an axis that lies in the plane of the crystal and is normal to the laser scanning direction. This paper reports on the fabrication of Sb 2 S 3 two-dimensional (2D) RLS crystals on the surface of 16SbI 3 -84Sb 2 S 3 glass, as a model example: individual RLS crystal lines are joined together using "stitching" or "rastering" as two successful protocols. The electron back scattered diffraction mapping and scanning Laue X-ray microdiffraction of the 2D RLS crystals show gradual rotation of lattice comprising of two components, one along the length of each line and another normal to this direction. The former component is determined by the rotation of the first line of the 2D pattern, but the relative contribution of the last component depends on the extent of overlap between two successive lines. By the appropriate choice of initial seed orientation and the direction of scanning, it is possible to control the lattice rotation, and even to reduce it down to 5 for a 50 × 50 μm 2 2D pattern of Sb 2 S 3 crystal.

36 MATERIALS SCIENCE↗

Synthesis and characterization of hydroxyapatite from fish bone waste

Waste fish bones is a problem stemming from activities in the field of fisheries and it has not been used optimally. Fish bones contain calcium as natural source that used to synthesize hydroxyapatite (HA). In this research, HA synthesized from waste fish bones as local wisdom in Semarang. The goal are to produce HA with cheaper production costs and to reduce the environmental problems caused by waste bones. The novelty of this study was using of local fish bone as a source of calcium and simple method of synthesis. Synthesis process of HA can be done through a maceration process with firing temperatures of 1000°C or followed by a sol-gel method with firing at 550°C. The results are analyzed using FTIR (Fourier Transform Infrared), XRD (X-Ray Diffraction) and SEM-EDX (Scanning Electron Microscopy-Energy Dispersive X-Ray). FTIR spectra showed absorption of phosphate and OH group belonging to HA as evidenced by the results of XRD. The average grain size by maceration and synthesized results are not significant different, which is about 69 nm. The ratio of Ca/P of HA by maceration result is 0.89, then increase after continued in the sol-gel process to 1.41. Morphology of HA by maceration results are regular and uniform particle growth, while the morphology of HA after the sol-gel process are irregular and agglomerated.

36 MATERIALS SCIENCE↗

Effect of the Boron Content on the Amorphization Process and Magnetic Properties of the Mechanically Alloyed Fe{sub 92−x}Nb{sub 8}B{sub x} Powders

The effect of the B content on the microstructural, structural, and magnetic properties of partially amorphous Fe{sub 92−x}Nb{sub 8}B{sub x} (x = 5, 10, 15, and 20) alloys has been investigated by means of scanning electron microscopy, X-ray diffraction, high and low-temperature extraction-type magnetometers. The XRD results reveal the formation of a nanocomposite structure where nanocrystalline bcc α-Fe and Fe{sub 2}B phases are embedded into an amorphous matrix. The FeB boride is observed for higher boron contents (x = 15 and 20), and the crystallite sizes are in the range of 7–24 nm. As the B content increases, the amorphous phase-relative proportion and coercivity increase, whereas the saturation magnetization decreases. An important magnetic hardening occurs by lowering the temperature from 400 to 5 K for x = 20% B. The variation of the Curie temperature can be attributed to the heterogeneity of the amorphous matrix.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Fast and low-cost method to fabricate large-area superhydrophobic surface on steel substrate with anticorrosion and anti-icing properties

A facile and quick fabrication method was proposed to prepare superhydrophobic surfaces on iron substrate by chemical immersion and subsequent stearic acid modification. The association between wettability and surface morphology was studied through altering the copper ion concentration and immersion time. Surface tension instrument, scanning electron microscopy, x-ray diffraction, x-ray photoelectron spectroscopy, and electrochemical workstation were used to characterize the wettability, physical morphology, chemical composition, and corrosion resistance ability of the prepared film. Results showed that both the rough micro/nanostructures and low surface energy material play critical roles in surface wettability. The superhydrophobic film achieved a better anticorrosion property compared to barrier iron by analysis of open circuit potential, potentiodynamic polarization curves, and Nyquist plots. In addition, the superhydrophobic surface showed excellent performance of acid and alkali resistance, anti-icing, and self-cleaning through a series of environmental tests. This study provides a valid method for quick-preparation of the stable superhydrophobic surfaces, which has a promising application in steel buildings and facilities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Electron-bombarded 〈110〉-oriented tungsten tips for stable tunneling electron emission

A clean tungsten (W) tip apex with a robust atomic plane is required for producing a stable tunneling electron emission under strong electric fields. Because a tip apex fabricated from a wire by aqueous chemical etching is covered by impurity layers, heating treatment in ultra-high vacuum is experimentally known to be necessary. However, strong heating frequently melts the tip apex and causes unstable electron emissions. We investigated quantitatively the tip apex and found a useful method to prepare a tip with stable tunneling electron emissions by controlling electron-bombardment heating power. Careful characterizations of the tip structures were performed with combinations of using field emission I–V curves, scanning electron microscopy, X-ray diffraction (transmitted Debye-Scherrer and Laue) with micro-parabola capillary, field ion microscopy, and field emission microscopy. Tips were chemically etched from (1) polycrystalline W wires (grain size ∼1000 nm) and (2) long-time heated W wires (grain size larger than 1 mm). Heating by 10-40 W (10 s) was found to be good enough to remove oxide layers and produced stable electron emission; however, around 60 W (10 s) heating was threshold power to increase the tip radius, typically +10 ± 5 nm (onset of melting). Further, the grain size of ∼1000 nm was necessary to obtain a conical shape tip apex.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Microstructural, Magnetic, and Nanoindentation Studies of the Ball-Milled Ti80Ni20 Alloy

Nanostructured Ti{sub 80}Ni{sub 20} material was elaborated by mechanical alloying from pure Ti and Ni powders in a planetary ball-mill P7 under argon atmosphere at ambient temperature. Morphological, microstructural, magnetic, and nanoindentation properties were studied using scanning electron microscopy, X-ray diffraction, magnetic measurements, and nanoindentation test. The morphological observations show the predominance of the welding phenomenon during the milling process. The Rietveld refinement of the X-ray diffraction pattern reveals, after 4 h of milling, the formation of the disordered hcp-Ti (Ni) solid solution in addition to elemental hcp-Ti and fcc-Ni. On further milling (20 h), the interdiffusion between Ti and Ni atoms is evidenced by the formation of disordered hcp-Ti (Ni) and fcc-Ni (Ti) solid solutions. The saturation magnetization and coercivity values are about of 159.8 emu/g and 80.79 Oe, respectively, after 20 h of milling. M{sub r}/M{sub s} ratio indicates the existence of small magnetic particles which are typically single domains (M{sub r}/M{sub s} 0.1–0.5) and/or multidomain (M{sub r}/M{sub s} < 0.1). Nanohardness values of the sintered powders fluctuates between 1.53 and 5.98 GPa while those of the elastic modulus varies in the range 130.73 to 164.53 GPa.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Magnetic and magneto elastic properties of cobalt ferrite ceramic compacted through cold isostatic pressing

Nano crystalline CoFe{sub 2}O{sub 4} powder was prepared by combustion synthesis method. As synthesized powder was calcined at an appropriate condition to remove the impurities and to promote phase formation. Phase pure CoFe{sub 2}O{sub 4} powder was pressed into cylindrical rod at an applied pressure of 200 MPa using a cold isostatic pressing. Sintering of the green compact at 1350°c for 12 hrs resulted in sintered cylindrical rod with ~85% of the theoretical density. Single phase cubic spinel structure was observed in the powder x-ray diffraction pattern of the sintered pellet. Scanning electron micrographs (SEM) of the as sintered pellet revealed the microstructure to be composed of ferrite grains of average size ~4 µm. Saturation magnetization of 72 emu/g and coercivity of 355 Oe were observed for cobalt ferrite sample. The magnetostriction was measured on a circular disc (12 mm diameter and 12 mm length) with the strain gauge (350 Ω) mounted on the flat surface of the circular disc. Magnetostriciton of 180 ppm and strain derivative of 1 × 10{sup −9} m/A were observed for the sintered CoFe{sub 2}O{sub 4} sample.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Study on Texture Evolution and Shear Behavior of an Al/Ni/Cu Composite

The microstructure, texture, and mechanical properties of the Al/Ni/Cu composite during various accumulative roll bonding (ARB) cycles were studied using optical microscopy, scanning electron microscopy, x-ray diffraction, shear punch test, and hardness test. In addition, ImageJ software and Rietveld software were used in order to study microstructure and dislocation density variations, respectively. It was found that Ni and Cu layers were fractured and distributed in the Al matrix due to differences in their mechanical properties. Fracture and distribution of Cu and Ni particles after cycle five led to the alteration of the composite structure from a layered to a particle-reinforced structure. ARB process leads to the formation of strong orientation along the β-fiber and also to pronounced copper and dillamore components in both Al and Cu phases. Furthermore, the shear yield stress and ultimate shear strength of the composite increased as the ARB process advanced; however, shear elongation presented a non-uniform variation. Investigation of the fracture surfaces revealed that the mechanical properties of the composite are affected not only by the strain hardening of the Cu layer, but also by the structural change in the composite during the initial ARB cycles. During the last stages of the process, however, changes in mechanical properties were mostly governed by reinforcement particles serving as strain concentration zones and the strain hardening of the Al matrix.

36 MATERIALS SCIENCE↗

Structural Characterization and Magnetic Properties of SrCo{sub 2}Fe{sub 16}O{sub 27} Hexaferrite Synthesized by Citric Acid Sol-Gel Method

The W -type SrCo{sub 2}Fe{sub 16}O{sub 27} (SCFO) hexagonal ferrite samples were prepared by the sol-gel method using metal nitrate as raw material, citric acid as complexing agent, and water as solvent. The effects of different sintering temperatures and holding times on the phase composition and morphology properties were explored in detail by using the X-ray diffractometer and field emission scanning electron microscope. The X-ray diffraction, microstructure, and magnetic performance of most optimum sintering temperature and holding time of preparing single-phase SCFO hexagonal ferrite were investigated. The experimental results indicate that the best optimum sintering temperature and holding time of SCFO hexagonal ferrite are 1280 °C and 4 h, respectively. Field emission scanning electron microscopy results indicate that the size of the particles is about 5–10 μ m. The result of magnetic measurement shows that SCFO hexagonal ferrite exhibits the soft magnetic property and the Curie temperature (T{sub C}) is ∼ 850 K. Furthermore, by analyzing the Arrott plot, the phase transition near the T{sub C} is a secondary phase transition.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A study on spherical particles in Al65Cu20Fe15 alloy prepared by arc melting

Highlights: • Spherical particles and facets were found. • Spherical particles consist of quasicrystalline grains embedded in single crystal matrix. • Facets were found on the surface of spherical particles, which can be classified to three types. • A model for the formation of spherical particles is suggested. • Reasons for the formation of facets are discussed. - Abstract: Al-Cu-Fe alloys are important due to reports that stable icosahedral quasicrystalline phase with composition in the vicinity of Al{sub 65}Cu{sub 20}Fe{sub 15} can be prepared. However, it has been widely reported that the as-prepared alloy, very often by arc-melting, is porous, consisting of particles with different morphologies. Among these, one type of particles of a spherical shape is considered as pure cubic β phase in previous reports. In this research, this spherical particle was studied using a Scanning Electron Microscope, Energy Dispersive X-ray Spectroscopy, Transmission Electron Microscope, and Electron Diffraction. It was found that the particles are not single phase, consisting of icosahedral quasicrystalline grains embedded inside single crystal matrix of τ phase. Additionally, there are places where the τ phase appears to have out-most layer enriched in Cu. The surface of the particles is faceted and the facets can be classified to three types according to their detailed structures. A close examination and analysis led to the conclusion that these three types are parallel to the atomic planes of {1 1 0}, {1 1 1}, and {1 0 0}, respectively. A model for the spherical particle formation is suggested and the reasons for the formation of facets are discussed. This report is valuable in clarifying some discrepancies in previous reports, and in understanding the phase development in an Al-Cu-Fe alloy system.

36 MATERIALS SCIENCE↗

Glass-bonded iodosodalite waste form for immobilization of 129I

Immobilization of radioiodine (e.g., 129I, 131I) is an important need for current and future nuclear fuel cycles. For the current work, iodosodalite [Na8(AlSiO4)6I2] was synthesized hydrothermally from metakaolin, NaI, and NaOH. Following hydrothermal treatment, dried unwashed powders were used to make glass-bonded iodosodalite waste forms by heating pressed pellets at 650, 750, or 850 °C with two different types of sodium borosilicate glass binders, i.e., NBS-4 and SA-800. These heat-treated specimens were characterized with X-ray diffraction, Fourier-transform infrared spectroscopy, scanning electron microscopy, energy dispersive spectroscopy, thermal analysis, porosity and density measurements, neutron activation analysis, and inductively-coupled plasma mass spectrometry. The pellets mixed with 10 mass% of NBS-4 or SA-800 and heat-treated at 750 °C contained relatively high percentage iodine retention (~44-47 % of the maximum iodine loading) with relatively low porosities, while other pellets with higher percentages iodine retention either contained higher porosity or were not completely sintered. ASTM C1308 chemical durability tests of monolithic specimens showed a large initial release of Na, Al, Si, and I on the first day, possibly from water-soluble salt crystals or non-durable amorphous phases. Release rates of Na and Si were higher than for Al and I, probably due to a poorly durable Na-Si-O phase from the glass bonding matrix. The cumulative normalized release of iodine was 12.5 g m-2 for the first 10 1-d exchanges, suggestive of coherent dissolution. The average release rate from 10-24 days during the 7-d exchange intervals was 0.2336 g m-2 d-1.

sodalite, iodosodalite, waste forms, iodine↗

Direct observations of crystal defects in polycrystalline diamond

Highlights: • Electron channeling contrast imaging of crystal defects in polycrystalline diamond • Introducing acid etching as a novel protocol for diamond surface preparation • Characterization of {111} twins, {111} stacking faults and {111} helical dislocations in diamond using ECCI and EBSD - Abstract: Crystal defects are abundant in synthetic diamond produced by chemical vapor deposition (CVD). We present the first images of crystal defects in a bulk polycrystalline CVD diamond sample using general electron channeling contrast imaging (ECCI) in a field emission scanning electron microscope (FE-SEM). For enhancement of channeling contrast of this material, we introduce a novel protocol for diamond surface preparation that involves acid etching. Using this protocol, we imaged three types of crystal defects including twins, stacking faults and dislocations. Each defect was identified based on its appearance in electron channeling contrast (ECC) micrographs. We analyzed grains containing twins and dislocations using electron backscatter diffraction (EBSD) crystal orientation mapping. We found a large population of grains that contained Σ3 type twins on {111} planes with a 60°<111> angle–axis pair of misorientation for twin boundaries. In addition, we identified {111} stacking faults and {111} helical dislocations. These observations are in agreement with reports of crystal defects in CVD diamond thin foils studied by a transmission electron microscope (TEM).

36 MATERIALS SCIENCE↗