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Results for “Electron Backscatter Diffraction”

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At least 991 records · Page 55
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

Free surface effects on the recrystallization of compressed, stable, Al-Mn single crystals

Highlights: • The free surface provokes high frequency nucleation. • The free surface and surface ‘quality’ do not modify the orientations of the recrystallized grains. • The misorientation relations across recrystallization front are similar for all sections of both orientations. The free surface effect on the grain crystallography and morphology during recrystallization has been studied in stable Goss {110}001 and brass {110}112 - oriented single crystals of Al-1%wt.Mn alloy. The samples were plane strain compressed up to a strain of about 0.5 to develop a homogeneous structure comprising two sets of symmetrical microbands and then lightly annealed. The variation of recrystallization after annealing was then analysed by optical microscopy and SEM/EBSD on different cross-sections. The results are discussed in terms of the misorientation angle and axis distributions. The free surface provokes high frequency nucleation leading to a small grain size compared to internal sections of the bulk sample. However, the free surface and surface ‘quality’ do not modify the orientations of the recrystallized grains, i.e. similar groups of recrystallized grain orientations were observed for all sections. This leads to a strong misorientation relation between deformed/recovered area orientations and the limited number of groups of recrystallized grain orientations, basically the same as those observed during bulk recrystallization of similar crystals.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Investigation of orientation inhomogeneities in polycrystalline materials by means of FEG-SEM, FIB, EBSD and 3-D reconstruction

The efficiency of different techniques application for the investigation of orientation inhomogeneities in polycrystalline materials was studied using FEG SEM-FIB dual beam station equipped with EBSD. It is shown that for the visualization of pearlitic ferrite fragments it is more appropriate to acquire the images in secondary electrons induced by Ga ions. At the same time for the visualization of nano-sized particles it is more prospective to use images in forward scatter electrons in combination with IQ maps. It is established that pearlitic ferrite fragments are not flat. Complicated spatial configuration of orientation inhomogeneities in pearlitic ferrite is shown by means of 3-d reconstruction. The features of ferrites aggregation are revealed depending on pearlitic ferrite fragmentation criterion. The existence of long-range misorientations in the aggregation area of proeutectoid and pearlitic ferrites is shown.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
NASA NTRSDate not supplied

The Zircon-Reidite Shock Transformation: A Tem Study of Reidite Produced at A Newly Established 21.2 GPa Shock Pressure Threshold

The high-pressure polymorph of zircon (Zr2SiO4) is reidite, a phase with the scheelite structure that was first discovered to form at ca. 12 GPa in static high-pressure experiments [1]. Reidite was subsequently found to occur in naturally shocked zircons from several terrestrial impact localities [2,3], as well as in shock recovery-reverberation experiments performed above 20 GPa [4]. The nature and distribution of reidite occurrences in terrestrial impact localities has pointed to its potential use as a shock pressure indicator, as well as to the importance of understanding its age-reset effects in zircon geochronology [3]. In this study we have used coordinated SEM/Electron Backscatter Diffraction (EBSD) and Field-Emission Scanning Transmission Electron Microscopy (FE-STEM) to study the micro- and nanostructure of reidite and its shocked zircon host produced at 21.2 GPa under experimental shock recovery/reverberation conditions [5]. Our results document the TEM microstructure of reidite formed at a 21.2 GPa experimental shock pressure that is significantly lower than that observed in previous studies [4]. At these conditions the sample developed a diverse set of microstructures that have not been previously documented on the TEM scale.

shock metamorphism↗
DOE OSTI2012

Atmospheric-Pressure Chemical Vapor Deposition of Iron Pyrite Thin Films

Iron pyrite (cubic FeS{sub 2}) is a promising candidate absorber material for earth-abundant thin-film solar cells. In this report, single-phase, large-grain, and uniform polycrystalline pyrite thin films are fabricated on glass and molybdenum-coated glass substrates by atmospheric-pressure chemical vapor deposition (AP-CVD) using the reaction of iron(III) acetylacetonate and tert-butyl disulfide in argon at 300 C, followed by sulfur annealing at 500--550 C to convert marcasite impurities to pyrite. The pyrite-marcasite phase composition depends strongly on the concentration of sodium in the growth substrate and the sulfur partial pressure during annealing. Phase and elemental composition of the films are characterized by X-ray diffraction, Raman spectroscopy, Auger electron spectroscopy, secondary ion mass spectrometry, Rutherford backscattering spectrometry, and X-ray photoelectron spectroscopy. The in-plane electrical properties are surprisingly insensitive to phase and elemental impurities, with all films showing p-type, thermally activated transport with a small activation energy ({approx}30 meV), a room- temperature resistivity of {approx}1 {Omega} cm, and low mobility. These ubiquitous electrical properties may result from robust surface effects. These CVD pyrite thin films are well suited to fundamental electrical studies and the fabrication of pyrite photovoltaic device stacks.

14 SOLAR ENERGY↗
DOE OSTI2015

Ge/GeSn heterostructures grown on Si (100) by molecular-beam epitaxy

The growth of GeSn layers by molecular-beam epitaxy on Si (100) wafers coated with a germanium buffer layer is investigated. The properties of the fabricated structures are controlled by reflection high-energy electron diffraction, atomic-force microscopy, X-ray diffractometry, Rutherford backscattering, and Raman scattering. It is shown that GeSn layers with thicknesses up to 0.5 μm and Sn molar fractions up to 0.073 manifest no sign of plastic relaxation upon epitaxy. The lattice constant of the GeSn layers within the growth plane is precisely the same as that of Ge. The effect of rapid thermal annealing on the conversion of metastable elastically strained GeSn layers into a plastically relaxed state is examined. Ge/GeSn quantum wells with Sn molar fraction up to 0.11 are obtained.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Thermoelectric transport properties of diamond-like Cu{sub 1−x}Fe{sub 1+x}S{sub 2} tetrahedral compounds

Polycrystalline samples with the composition of Cu{sub 1−x}Fe{sub 1+x}S{sub 2} (x = 0, 0.01, 0.03, 0.05, 0.1) were synthesized by a melting-annealing-sintering process. X-ray powder diffraction reveals all the samples are phase pure. The backscattered electron image and X-ray map indicate that all elements are distributed homogeneously in the matrix. The measurements of Hall coefficient, electrical conductivity, and Seebeck coefficient show that Fe is an effective n-type dopant in CuFeS{sub 2}. The electron carrier concentration of Cu{sub 1−x}Fe{sub 1+x}S{sub 2} is tuned within a wide range leading to optimized power factors. The lattice phonons are also strongly scattered by the substitution of Fe for Cu, leading to reduced thermal conductivity. We use Debye approximation to model the low temperature lattice thermal conductivity. It is found that the large strain field fluctuation introduced by the disordered Fe ions generates extra strong phonon scatterings for lowered lattice thermal conductivity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Vickers Microhardness Studies for SmBa{sub 2}Cu{sub 3}O{sub 7-δ} Added with NiO Nanosized Particles

The effect of nanosized particles NiO addition on the Vickers microhardness of polycrystalline SmBa{sub 2}Cu{sub 3}O{sub 7-δ} was investigated. Various amounts of nanosized particles NiO (x = 0.00, 0.02, 0.04, 0.08, and 0.12 wt%) were added to SmBa{sub 2}Cu{sub 3}O{sub 7-δ} prepared by the solid-state reaction method. Sample characterizations were carried out using X-ray powder diffraction (XRD), particle induced X-ray emission (PIXE), Rutherford backscattering (RBS), and scanning electron microscopy (SEM). The nanosized particle addition does not influence the orthorhombic structure of SmBa{sub 2}Cu{sub 3}O{sub 7-δ}, whereas it affects the oxygen content δ. The electrical and mechanical properties of (NiO){sub x}SmBa{sub 2}Cu{sub 3}O{sub 7-δ} samples were measured using four-standard probe technique and Vickers microhardness in order to investigate the effect of NiO nanosized particles on superconducting transition temperature and Vickers microhardness number H{sub v}. The Vickers microhardness data were analyzed using Hays and Kendall (HK), elastic plastic deformation (EPD), and modified proportional specimen resistance (MPSR) models. The analysis showed that the MPSR model was found to be the best to describe the behavior of H{sub v}.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2014

Atomic layer deposition of bismuth oxide using Bi(OCMe{sub 2}{sup i}Pr){sub 3} and H{sub 2}O

Bismuth oxide thin films were deposited by atomic layer deposition using Bi(OCMe{sub 2}{sup i}Pr){sub 3} and H{sub 2}O at deposition temperatures between 90 and 270 °C on Si{sub 3}N{sub 4}, TaN, and TiN substrates. Films were analyzed using spectroscopic ellipsometry, x-ray diffraction, x-ray reflectivity, high-resolution transmission electron microscopy, and Rutherford backscattering spectrometry. Bi{sub 2}O{sub 3} films deposited at 150 °C have a linear growth per cycle of 0.039 nm/cycle, density of 8.3 g/cm{sup 3}, band gap of approximately 2.9 eV, low carbon content, and show the β phase structure with a (201) preferred crystal orientation. Deposition temperatures above 210 °C and postdeposition anneals caused uneven volumetric expansion, resulting in a decrease in film density, increased interfacial roughness, and degraded optical properties.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

A transmission Kikuchi diffraction study of cementite in a quenched and tempered steel

This is the first transmission Kikuchi diffraction (TKD) study to report the indexing of nano-sized cementite as distinct structures and its orientation relationship with the body-centered cubic matrix in a quenched and tempered steel. Crystallographic analysis via TKD and selected area diffraction returned the well-known Bagaryatskii and Isaichev orientation relationships. However, the indexing of nano-sized cementite via TKD was sensitive to the thickness of the electron transparent region such that TEM remains the most precise method to characterise such precipitates. - Highlights: • Nano-sized cementite in a QT steel has been investigated by TKD and TEM. • Cementite has been indexed as distinct structures via TKD. • Crystallographic analysis returned the Bagaryatskii and Isaichev ORs. • Success of TKD is sensitive to the thickness of the electron transparent region. • TEM remains the most precise technique to characterise nano-sized precipitates.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Grinding-induced metallurgical alterations in the binder phase of WC-Co cemented carbides

The metallic binder phase dictates the toughening behavior of WC-Co cemented carbides (hardmetals), even though it occupies a relative small fraction of the composite. Studies on deformation and phase transformation of the binder constituent are scarce. Grinding represents a key manufacturing step in machining of hardmetal tools, and is well-recognized to induce surface integrity alterations. In this work, metallurgical alterations of the binder phase in ground WC-Co cemented carbides have been assessed by a combination of electron back scattered diffraction and transmission electron microscopy techniques. The Co-base binder experiences a martensitic phase transformation from fcc to hcp crystal structure, predominantly in the first 5 μm below the surface. The hcp fraction decreases gradually along a depth of 10 μm. Surface Co displays severe plastic deformation under the highest strain, resulting in formation of nanocrystalline grains in the first micrometer below the surface. Microstructural refinement within the binder phase is observed even at greater depth. Stacking faults were detected in most of the refined grains. The metallurgical alterations of the binder phase modify the local stress distribution during grinding, which affects the discerned subsurface microcracking. The resulting residual stress profile is the sum of multiple subsurface changes, such as phase transformation, severe plastic deformation and grain refinement, where it is discerned that the depth profile of the transformed hcp-Co fraction coincides with the grinding-induced residual stress profile.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Corrosion Behavior of Nano-/Ultrafine-Grained Al-0.2 wt.% Sc Alloy Produced by Accumulative Roll Bonding (ARB)

The corrosion behavior of the Al-0.2 wt.% Sc alloy fabricated by the accumulative roll bonding (ARB) process in a 3.5 wt.% NaCl solution was studied using the electrochemical impedance spectroscopy and potentiodynamic polarization techniques. The effect of the microstructural parameters, such as dislocation density, texture, grain boundary, and lattice strain, on the corrosion behavior was also investigated in this study. The results demonstrated that the ARB process can significantly improve the corrosion resistance and modify the corrosion potential to attain higher positive potentials. In addition, the pitting corrosion changed into the lateral spreading of the pits at the seventh and tenth cycles of the ARB process with average grain size of 410 and 370 nm, respectively. The change in the fraction of the high-angle grain boundary during the ARB process is the most important parameter regarding the variation in corrosion type. The average grain size of 410 nm in seventh cycle, as the optimum average grain size, demonstrated the highest corrosion resistance.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2016

Structural and magnetic properties of ferrimagnetic ε-phase Mn 4 N and antiferromagnetic ζ-phase Mn10N thin films on MgO(001)

Single phase ε-Mn 4 N and ζ-Mn 10 N thin films are grown on MgO(001) using molecular beam epitaxy. The films are identified and characterized using reflection high-energy electron diffraction, x-ray diffraction, back scattered electron scanning electron microscopy, atomic/magnetic force microscopy and Rutherford backscattering spectrometry. These films are found to be highly smooth with root-mean-squared roughnesses 3.39 nm and below. The quality of ε-Mn 4 N grown is strongly dependent on substrate temperature during growth. Epitaxial growth of substantial grains composed of the antiferromagnetic η-phase Mn 3 N 2 side by side with ferrimagnetic ε-phase grains is observed when growth temperature is below 480 °C. Ising domains isolated within areas roughly 0.5 μm across are observed in the ferrimagnetic ε-phase grains of samples consisting of a mix of η- and ε-phase grains. Magnetic domains following semi-continuous paths, which are 0.7–7.2 μm across, are observed in single phase ε-Mn4N. Measurements of the ζ-phase detail the structure and magnetism of the material as high Mn content γ-type ζ-phase with a regular surface corrugation along the [100]-direction and antiferromagnetic.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Powder metallurgy processing and deformation characteristics of bulk multimodal nickel

Spark plasma sintering was used to process bulk nickel samples from a blend of three powder types. The resulting multimodal microstructure was made of coarse (average size ∼ 135 μm) spherical microcrystalline entities (the core) surrounded by a fine-grained matrix (average grain size ∼ 1.5 μm) or a thick rim (the shell) distinguishable from the matrix. Tensile tests revealed yield strength of ∼ 470 MPa that was accompanied by limited ductility (∼ 2.8% plastic strain). Microstructure observation after testing showed debonding at interfaces between the matrix and the coarse entities, but in many instances, shallow dimples within the rim were observed indicating local ductile events in the shell. Dislocation emission and annihilation at grain boundaries and twinning at crack tip were the main deformation mechanisms taking place within the fine-grained matrix as revealed by in-situ transmission electron microscopy. Estimation of the stress from loop's curvature and dislocation pile-up indicates that dislocation emission from grain boundaries and grain boundary overcoming largely contributes to the flow stress. - Highlights: • Bulk multi-modal Ni was processed by SPS from a powder blend. • Ultrafine-grained matrix or rim observed around spherical microcrystalline entities • Yield strength (470 MPa) and ductility (2.8% plastic strain) were measured. • Debonding was found at the matrix/microcrystalline entity interfaces. • In-situ TEM showed twinning, dislocation emission and annihilation at grain boundaries.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Investigation of deformation micro-mechanisms in nickel consolidated from a bimodal powder by spark plasma sintering

Bulk polycrystalline nickel compact was processed by spark plasma sintering from heterogeneous powder consisting of a mixture of nanometer and micrometer sized particles. The consolidated samples inherited the bimodal structure of the starting powder and was composed of ~ 55 vol.% coarse-grained (with the grain size larger than 1 μm) and ~ 45 vol.% ultrafine-grained (with an average grain size of ~ 550 nm) components. The deformation mechanisms were established by EBSD, X-ray line profile analysis and in-situ TEM observations. In the ultrafine-grained volume, the deformation occurred mainly through the activation of dislocation sources emitting full or partial dislocation either from grain interior or grain boundaries. Besides dislocation activity, rolling and sliding of nanograins were also observed during deformation by in-situ transmission electron microscopy, which have a considerable contribution to the observed high strain rate sensitivity of the bimodal microstructure. The cracks formed during deformation easily propagated in the nanograin regions due to the weaker particle bonding caused by the relatively high fraction of native oxide layer on the surface of the initial nanoparticles. - Highlights: • Bulk bimodal polycrystalline Ni was processed by SPS from a heterogeneous powder. • High SRS of the flow stress was observed which enhanced ductility and strength. • In-situ TEM revealed dislocation sources inside and at the boundaries of UFGs. • Twinning, partial dislocation and NG rolling were observed at crack tip vicinity. • The high SRS pertained to both dislocation activity in CG and NG rolling.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2016

Microstructure and wear characterization of aluminum matrix composites reinforced with industrial waste fly ash particulates synthesized by friction stir processing

Fly ash (FA) is a waste product of coal combustion in thermal power plants which is available in massive quantities all over the world causing land pollution. This paper reports the characterization of AA6061 aluminum matrix composites (AMCs) reinforced with FA particles synthesized using friction stir processing (FSP). The volume fraction of FA particles was varied from 0 to 18 in steps of 6. The prepared AMCs were characterized using optical microscopy (OM), scanning electron microscopy (SEM) and electron backscattered diagram (EBSD). The wear rate was estimated using a pin-on-disc wear apparatus. FA particles were observed to be distributed homogeneously in the AMC irrespective of the location within the stir zone. The EBSD micrographs revealed remarkable grain refinement in the AMC. The incorporation of FA particles enhanced the microhardness and wear resistance of the AMC. The strengthening mechanisms of the AMC were discussed and correlated to the observed microstructures. The wear mechanisms were identified by characterizing the wear debris and worn surfaces. - Highlights: •Industrial waste fly ash was used to produce aluminum matrix composites. •Friction stir processing was used to produce AA6061/Fly Ash composite. •Fly ash particles refined the grains of aluminum matrix. •Fly ash particles enhanced the hardness and wear resistance. •Successful utilization of fly ash to make aluminum composites reduces land pollution.

36 MATERIALS SCIENCE↗
DOE OSTI2016

Ghost microstructure evolution and identification in the coarse grain heat affected zone of 2.25Cr-1Mo-V-Ti steel using tint etching

Microstructural characteristics of the CGHAZ (coarse grained heat affected zone) made of the 2.25Cr-1Mo-V-Ti material for the thermal power plant boiler tube were discussed using the technique of tint etching. To conduct the micro structural characterization, the sample on which CGHAZ was produced by using a high temperature thermal cycle simulator, Gleeble 3500 equipment was used for comparative analyses using the existing Nital etching (ASTM E407-74) and the alkaline etching (ASTM E40785). The latter was used to observe a specific phase. For the microstructure on which the alkaline etching was experimented, the shape of a black strip (Ghost microstructure) in a few microns was observed, which was not observed from the Nital etching. It was found from the phase identifications based EPMA, EBSD and TEM experiments that the image of the black strip in a few microns represented the alpha phase in which C, Cr and Mo became segregated. In addition, it was verified that austenite and M{sub 23}C{sub 6} phase were present around the segregated zone. Based on such results, the mechanism by which the image of the black strip in a few microns was formed at the CGHAZ. In this study, we have investigated the mechanism of the appeared black strip in the CGHAZ. - Highlights: •Ghost microstructure was observed which was not observed from the nital etching. •Ghost microstructure has high concentrations of carbon and molybdenum than matrix. •Schematic illustration proposed of why Ghost microstructure was generated. •Ghost microstructure caused by partial dissolution of M{sub 23}C{sub 6} precipitation.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure of titanium on complex deformation paths: Comparison of ECAP, KOBO and HE techniques

Highlights: • Method for producing CP titanium rods for medical implants is searched. • Three processing methods producing ultra-fine grain titanium are compared. • Microstructure and textures are examined and analysed. • Mechanical characteristics are determined based on microhardness and tensile tests. • Hydrostatic extrusion (HE) leads to the best properties of titanium rods for medical implants. - Abstract: In this work samples of commercial purity grade 2 titanium were severely deformed by three different extrusion techniques: equal-channel angular pressing (ECAP), extrusion through oscillating die (KOBO), and hydrostatic extrusion (HE). Resulting microstructures and mechanical properties of processed titanium samples are studied and compared with regard to potential application as a material for dental implants. The obtained results demonstrate the effect of different strain paths, involved by three applied deformation methods, on microstructure refinement, mechanical properties and textures of the studied material. Heterogeneous microstructures with bimodal grain size distributions are observed for all deformation techniques in the examined material, however differences in their internal structures and grain boundary distributions point to different grain refinement mechanisms. The fraction of ultra-fine grains is the highest in titanium deformed by HE. Also the internal grain fragmentation is the most important after HE deformation. This leads to the best mechanical and microstructural properties obtained in this type of deformation. Consequently, the HE process seems to be very interesting for production of material for medical implants.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Analyzing the microstructural evolution and hardening response of an Al-Si-Mg casting alloy with Cr addition

Highlights: • The formation of β-Al{sub 5}FeSi intermetallics was suppressed since impurity Fe has been consumed by Al{sub 13}Cr{sub 4}Si{sub 4} intermetallics; • A large number of Al{sub 13}Cr{sub 4}Si{sub 4} dispersoids were observed in Al dendrites in the as-quenched and aged alloy; • The precipitation of Cr-bearing dispersoids harden the as-quenched alloy by over 10HV; • The current thermodynamic database underestimate the solubility of Fe in Al{sub 13}Cr{sub 4}Si{sub 4} intermetallics during solidification simulation. - Abstract: Chromium is added to Al-Si based casting alloys for the mitigation of die soldering. In the present work, EBSD, EDS and TEM characterizations are combined with thermodynamic simulations to study the microstructural evolution and hardening response of an Al-Si-Mg-Cr casting alloy during heat treatments. It is shown that the Fe-containing intermetallic compounds formed in the inter-dendritic region were acicular π-Al{sub 8}(Fe, Cr)Mg{sub 3}Si{sub 6} phase and polyhedral Al-(Cr, Fe)-Si phase which is structurally similar to face-centered cubic Al{sub 13}Cr{sub 4}Si{sub 4}. The polyhedral Al-(Cr, Fe)-Si intermetallics that crystallized prior to β-Al{sub 5}FeSi consumed impurity Fe, suppressing the formation of β phase during gravity die casting process. Also, Cr-addition enables the precipitation of nano-scale Cr-bearing dispersoids in Al dendrite during solution treatment at 813 K. Hardness increment of over 10 HV can be induced by the Cr-bearing dispersoids for as-quenched alloy. Though the dispersoids have a moderate hardening effect on the as-quenched alloy, they may impair the ageing hardening response by acting as heterogeneous nucleation sites for coarse Mg-Si rods and Si particles when quenching into water at 338 K.

36 MATERIALS SCIENCE↗