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Results for “Electron Backscatter Diffraction”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 1,063 records · Page 59
All sourcesNASA NTRSDOE OSTI
DOE OSTI2018

The influence of power spinning and annealing temperature on microstructures and properties of Cu-Sn alloy

Highlights: • The strengthening effect of power spinning is mainly achieved by strengthening fine grains and dislocations. • Twins formed by the aggregation and overlapping of stacking faults grow and widen • In power spinning of Cu-Sn alloy, plastic deformation is primarily powered by dislocation sliding. - Abstract: Electron back scatter diffraction pattern (EBSD), metallographic microscope (OM) and transmission electron microscope (TEM) are used to analyze the microstructural state of the Cu-Sn alloy before and after power spinning and annealing. The results show that after power spinning, the α phase grains are refined and gradually evolve into small and fine α{sub II} and deformed α{sub III} crystal grains, with an average grain size of about 2.2 μm. Work hardening results in massive network-like subgrain boundaries distributed in power spinning microstructure. Annealing at 400 °C contributes to the formation of dislocation cells and stacking faults, and high-angle grain boundaries (HABS) start to migrate and slide. After the formation of less defective equiaxed grains at 500 °C, twins continue to grow and widen based through continuous accumulation of stacking faults. Further testing of mechanical properties reveals that power spinning is conducive to the improvement of mechanical properties of Cu-Sn alloy.

36 MATERIALS SCIENCE↗
NASA NTRS1974

Structure and properties of solid surfaces

Difficulties in experimental studies of crystalline surfaces are related to the fact that surface atoms have an intrinsic tendency to react with their environment. A second problem is connected with the effective thickness of surfaces, which ranges from one to several atom layers. The phenomenology of surface interactions with gases are considered, taking into account physical adsorption, chemisorption, and the oxidation of surfaces. Studies of the surface structure are discussed, giving attention to field emission microscopy, field-ion microscopy, electron diffraction techniques, Auger spectroscopy, scanning electron microscopy, electron probe microanalysis, ion microprobe methods, and low-energy backscattering spectroscopy. Investigations of semiconductor surfaces are also described.

Gatos, H. C.↗
DOE OSTI2020

Epitaxial growth of rock salt MgZrN 2 semiconductors on MgO and GaN

Ternary nitride compound semiconductors have attracted recent attention as electronic materials since their properties can be tuned by cation stoichiometry and ordering. A recently discovered example is MgZrN 2 , a ternary analog to the rock salt semiconductor ScN. MgZrN 2 has a larger bandgap and stronger dielectric response than the binary compound. Polycrystalline thin films of MgZrN 2 have been studied, but demonstration of high-quality growth is still required to establish its suitability for technological applications. Here, we report on epitaxial growth of MgZrN 2 thin films on (100) and (111) MgO substrates and (001) GaN templates. The MgZrN 2 composition is confirmed by Rutherford backscattering spectrometry, showing no oxygen in the film except for a thin surface oxide layer. Epitaxial growth results in MgZrN 2 with x-ray diffraction rocking curves with a full-width at half-maximum in the range of 0.3–3.0°, depending on the substrate. Transmission electron microscopy analysis of the MgZrN 2 film grown on a (111) MgO substrate confirms epitaxial growth and shows a sharp film/substrate interface. In-plane temperature-dependent Hall effect measurements show that the material is an n-type semiconductor with a relatively high concentration ( n 300K ≈ 10 19 –10 20 cm -3 ) of thermally activated electrons. Room-temperature transport measurements show a conductivity of 25 S cm -1 and a Seebeck coefficient of -80 μ V K -1 . Overall, these results provide an important step toward integration of rock salt MgZrN 2 with other technological nitrides for device applications.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Simulation Kinetics of Austenitic Phase Transformation in Ti+Nb Stabilized IF and Microalloyed Steels

In the present study, the influence of cooling rates (low to ultrafast) on diffusion controlled and displacive transformation of Ti-Nb IF and microalloyed steels has been thoroughly investigated. Mechanisms of nucleation and formation of non-equiaxed ferrite morphologies (i.e., acicular ferrite and bainitic ferrite) have been analyzed in details. The continuous cooling transformation behavior has been studied in a thermomechanical simulator (Gleeble 3800) using the cooling rates of 1-150 °C/s. On the basis of the dilatometric analysis of each cooling rate, continuous cooling transformation (CCT) diagrams have been constructed for both the steels to correlate the microstructural features at each cooling rate in different critical zones. In the case of the IF steel, massive ferrite grains along with granular bainite structures have been developed at cooling rates > 120 °C/s. On the other hand, a mixture of lath bainitic and lath martensite structures has been formed at a cooling rate of ~ 80 °C/s in the microalloyed steel. A strong dependence of the cooling rates and C content on the microstructures and mechanical properties has been established. The steel samples that were fast cooled to a mixture of bainite ferrite and martensite showed a significant improvement of impact toughness and hardness (157 J, for IF steel and 174 J for microalloyed steel) as compared to that of the as-received specimens (133 J for IF steel and 116 J for microalloyed steel). Thus, it can be concluded that the hardness and impact toughness properties are correlated well with the microstructural constituents as indicated by the CCT diagram. Transformation mechanisms and kinetics of austenitic transformation to different phase morphologies at various cooling rates have been discussed in details to correlate microstructural evolution and mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2026

Expanding the Zinc Precursor Toolbox: A Comparative Study of Precursors for Thermal ALD of ZnO Thin Films

Atomic layer deposition (ALD) of zinc oxide (ZnO) has been widely researched using diethyl zinc (DEZ)-based methods. The significant importance of thin films of ZnO as transparent conductive oxides (TCO) in optoelectronic devices and photovoltaics warrants examining alternative Zn precursors for ZnO ALD as potential replacements for the pyrophoric DEZ. In this study, we investigated three alternative Zn precursors: Zn(EEKI)2, Zn(DMP)2, ZnEt(HMDS), in the process development for high-quality ZnO thin films and compared them to DEZ. The ALD processes were studied using in situ spectroscopic ellipsometry. The properties of the ALD ZnO films were characterized using ex situ X-ray photoelectron spectroscopy (XPS), Rutherford backscattering spectrometry and nuclear reaction analysis (RBS/NRA), X-ray diffraction (XRD), atomic force microscopy (AFM), transmission electron microscopy (TEM), and ultraviolet-visible (UV/Vis) spectrophotometry. These measurements confirmed the formation of pure, stoichiometric, and polycrystalline ZnO films using all four Zn precursors. Although the selected precursors are chemically diverse Zn compounds, they all yielded saturating ALD processes and high-quality ZnO thin films at 200 °C. This study highlights the potential benefits of alternative zinc precursors in designing ALD processes for ZnO thin films.

Obenlüneschloß, Jorit↗
DOE OSTI2013

Variation of lattice constant and cluster formation in GaAsBi

We investigate the structural properties of GaAsBi layers grown by molecular beam epitaxy on GaAs at substrate temperatures between 220–315 °C. Irrespective of the growth temperature, the structures exhibited similar Bi compositions, and good overall crystal quality as deduced from X-Ray diffraction measurements. After thermal annealing at temperatures as low as 500 °C, the GaAsBi layers grown at the lowest temperatures exhibited a significant reduction of the lattice constant. The lattice variation was significantly larger for Bi-containing samples than for Bi-free low-temperature GaAs samples grown as a reference. Rutherford backscattering spectrometry gave no evidence of Bi diffusing out of the layer during annealing. However, dark-field and Z-contrast transmission electron microscopy analyses revealed the formation of GaAsBi clusters with a Bi content higher than in the surrounding matrix, as well as the presence of metallic As clusters. The apparent reduction of the lattice constant can be explained by a two-fold process: the diffusion of the excess As incorporated within As{sub Ga} antisites to As clusters, and the reduction of the Bi content in the GaAs matrix due to diffusion of Bi to GaAsBi clusters. Diffusion of both As and Bi are believed to be assisted by the native point defects, which are present in the low-temperature as-grown material.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Particle stimulated nucleation during dynamic and metadynamic recrystallisation of Ni-30%Fe-Nb-C alloy

For the first time, a combination of scanning transmission electron microscopy and electron back-scattering diffraction is used to elucidate the early stages of particle stimulated recrystallisation at Nb carbides in Ni-30wt.%Fe alloy subjected to high temperature plane strain compression. While particles with sizes even below 1 μm were found to induce dynamic or metadynamic recrystallisation, only a small fraction of coarse particles served as nucleation sites. - Highlights: • The early stages of particle stimulated recrystallisation at Nb carbides are elucidated • A combination of transmission electron microscopy and electron back scattering diffraction used • Particles below 1 μm size could induce dynamic or metadynamic recrystallization.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Influence of Thermomechanically Controlled Processing on Microstructure and Hydrogen Induced Cracking Susceptibility of API 5L X70 Pipeline Steel

The effect of different thermomechanical controlled processing routes on susceptibility of X70 pipeline steel to hydrogen induced cracking (HIC) have been studied. Two X70 pipeline steel specimens labelled WE and WD were investigated. These specimens have the same chemical composition, but they were processed with seperate thermomechanical treatments parameters. Microstructural examinations showed that WE consists of mainly acicular ferrite and polygonal ferrite, while WD consists of acicular ferrite and bainitic ferrite. After subjecting both specimens to hydrogen charging for 12 and 16 h in 0.2 M sulfuric acid and 3 g/L ammonium thiocyanate, early onset of HIC was observed in specimen WD. Post-hydrogen charging microstructural evaluation showed the nucleation of discontinuous cracks in WD after 12 h of charging. However, extended charging for up to 16 h resulted in HIC along the mid-thickness region of both specimens. Hydrogen diffusion across specimen WE was better than that of specimen WD. Therefore, hydrogen trapping at grain boundaries, banded deformed grains, inclusions and secondary phases such as martensite and cementite aided initiation and propagation of HIC in specimens. Nevertheless, the adverse effect of these features on HIC risks was more prominent in specimen WD compared to specimen WE. The Vickers microhardness values measured in WD (349.6 HV) and WE (307.4 HV) suggest that WD is harder than WE; and higher kernel average misorientation of 0.66° in WD than in WE (0.58°) shows higher dislocation density in WD. The results from slow strain rate tensile test confirmed that specimen WD was stronger and more susceptible to HIC than specimen WE. It was concluded that microstructural phases developed during thermomechanical processing improved strength in WD at the expense of its crack resistance, while WE with lower strength showed more ductility and higher resistance to HIC.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Characterization of high-temperature mechanical properties of plasma-cladded coatings with thermo-mechanical coupling

High temperature mechanical properties was detected here to study the failure and strengthening mechanism of the coating-substrate (cobalt-based coatings were fabricated on FV520B substrate) integral structure with thermo-mechanical coupling effects. Microstructure, phase composition, element distribution of the coatings was characterized by optical microscopy (OM), scanning electron microscopy (SEM), transmission electron microscope (TEM), electron back scattering diffraction (EBSD), X-ray diffraction (XRD), electron probe microanalysis (EPMA) and energy dispersive X-ray analysis (EDS). Results elucidate that fracture occurs in the coating for Co50 coating-substrate structure from 300 °C to 700 °C, but failure position transfer to substrate from coating at elevated temperatures with the addition of niobium and cerium oxide. Throughout, there is no crack originated from the interface. Fracture mechanism: the dislocation pile-up causes great stress concentration in the grain boundary, which results in the nucleation of the crack, and then the crack extends along the hard brittle Fe-Cr phase until the material fails. HRTEM shows the high density dislocation and the severe lattice distortion was formed during tensile deformation. On the macro level, the fracture tends to occur in the coarse dendrites region.

36 MATERIALS SCIENCE↗
DOE OSTI2015

Embedded Ge nanocrystals in SiO{sub 2} synthesized by ion implantation

200 nm thick SiO{sub 2} layers grown on Si substrates were implanted with 150 keV Ge ions at three different fluences. As-implanted samples were characterized with time-of-flight secondary ion mass spectrometry and Rutherford backscattering spectrometry to obtain depth profiles and concentration of Ge ions. As-implanted samples were annealed at 950 °C for 30 min. Crystalline quality of pristine, as-implanted, and annealed samples was investigated using Raman scattering measurements and the results were compared. Crystalline structure of as-implanted and annealed samples of embedded Ge into SiO{sub 2} matrix was studied using x-ray diffraction. No secondary phase or alloy formation of Ge was detected with x-ray diffraction or Raman measurements. Scanning transmission electron microscope measurements were done to get the nanocrystal size and localized information. The results confirmed that fluence dependent Ge nanocrystals of different sizes are formed in the annealed samples. It is also observed that Ge is slowly diffusing deeper into the substrate with annealing.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Fractal analysis of Mo and Nb effects on grain boundary character and hot cracking behavior for Ni-Cr-Fe alloys

Highlights: • Cross section of the weld with lower RHGB fractal dimension exhibited higher DDC susceptibility than the surface section. • Mo and Nb addition induced tortuous GB character to increase fractal dimension and improve cracking resistance. • GROD maps indicated that the local strain increased within the grains close to RGBs till cracking. • At 1050 °C deformation recrystallized grains nucleated adjacent to DDC and blocked the crack propagation. - Abstract: In this paper, two filler metals of alloy 690 were evaluated on their hot cracking resistance based on the fractal analysis of random high-angle grain boundary (RHGB) morphologies. A grain reference orientation deviation (GROD) map based on EBSD technique was conducted to investigate the polycrystalline strain distribution on different RHGB network. It was found that for the 52M weld metal, specimen from the cross section with straight dendritic GBs exhibited lower fractal dimension, showing higher DDC susceptibility than the specimen from the surface section with higher fractal dimension due to equiaxed grains with tortuous GBs. With Mo and more Nb adding to the filler metal 52MSS, smaller grains nucleated and fractal dimension of the RHGB network increased, thus the cracking resistance was greatly improved. The GROD results revealed that local strain commonly concentrated around RHGB at high temperatures, especially near long and straight RHGB. The dense and tortuous RHGB network, resulting in the higher fractal dimension, could bear a more uniform strain distribution and balance the deformation between GB and grains, leading to better performance on cracking resistance. Moreover, dynamic recrystallized grains were observed beside GBs and their amount increases where there was cracking at 1050 °C, especially for the 52MSS. As a result, crack propagation path was blocked and fractal dimension increased as well.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Assessment of diagenesis in archaeological human second metacarpal bones using the intensity of the small angle X-ray scattering D -period peak

Bone consists mainly of carbonated apatite (cAp) nanoplatelets embedded in a matrix of collagen fibrils. Earlier, high-energy small angle X-ray scattering (SAXS) studies of archaeological adult human second metacarpal bones (mc2) found collagen D-period peaks with high-intensity I D in specimens in which microcomputed tomography (microCT) showed little diagenesis and I D ~ 0 for specimens where microCT revealed severe diagenesis (Park et al. 2022 Int. J. Osteoarchaeol. 32, 170–181 (doi:10.1002/oa.3053); Stock et al. 2022 Int. J. Osteoarchaeol. 32, 120–131 (doi:10.1002/oa.3049)). Here, the present paper uses SAXS at beamline 1-ID, Advanced Photon Source, Argonne National Laboratory and other techniques to study a set of 10 mc2 from an early Medieval cemetery at Greding, Germany. We hypothesized that non-invasive measurement of I D would provide an accurate and rapid (approx. 6 min/specimen) assessment of diagenesis in archaeological mc2. Results of Raman spectroscopy, laboratory microCT and backscattered electron, reflected light and polarized transmitted light microscopies confirmed the SAXS determinations, but lattice parameter values from X-ray diffraction were uncorrelated with I D value. Age-at-death estimates placed the 10 mc2 in three age categories (young adult, middle adult, old adult): lattice parameters from X-ray diffraction were uncorrelated with age at death. Cross-sectional bone area fraction from microCT dropped noticeably for the older age cohort.

Raman spectroscopy↗
DOE OSTI2012

Structural and electrical studies of ultrathin layers with Si{sub 0.7}Ge{sub 0.3} nanocrystals confined in a SiGe/SiO{sub 2} superlattice

In this work, SiGe/SiO{sub 2} multi-layer (ML) films with layer thickness in the range of a few nanometers were successfully fabricated by conventional RF-magnetron sputtering at 350 deg. C. The influence of the annealing treatment on SiGe nanocrystals (NCs) formation and crystalline properties were investigated by Raman spectroscopy and grazing incidence x-ray diffraction. At the annealing temperature of 800 deg. C, where well defined SiGe NCs were observed, a thorough structural investigation of the whole ML structure has been undertaken by Rutherford backscattering spectroscopy, grazing incidence small angle x-ray scattering, high resolution transmission electron microscopy, and annular dark field scanning transmission electron microscopy. Our results show that the onset of local modifications to the ML composition takes place at this temperature for annealing times of the order of a few tens of minutes with the formation of defective regions in the upper portion of the ML structure. Only the very first layers over the Si substrate appear immune to this problem. This finding has been exploited for the fabrication of a defect free metal-oxide-semiconductor structure with a well-defined single layer of SiGe NCs. A memory effect attributed to the presence of the SiGe NCs has been demonstrated by high frequency capacitance-voltage measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Influence of crystal mosaicity on axial channeling effects and lattice site determination of impurities

Using the electron emission channeling and Rutherford backscattering/channeling techniques, the influence of the mosaicity of a thin film on the axial channeling of charged particles was investigated. It is found that crystal mosaicity leads to a broadening and a degradation of the experimental channeling effects. This phenomenon, which is shown to be of major importance when assessing the lattice site of impurities in a single crystal, can be modeled quantitatively by using the mosaic tilt and twist components derived from X-ray rocking curve scans. As a case study, we illustrate that our approach allows to accurately determine the lattice site of Er in AlN, despite the significant influence of mosaicity on the channeling measurements.

36 MATERIALS SCIENCE↗
DOE OSTI2012

RBS, XRR and optical reflectivity measurements of Ti-TiO{sub 2} thin films deposited by magnetron sputtering

Highlights: Black-Right-Pointing-Pointer The single-, bi- and tri-layered films of Ti-TiO{sub 2} deposited onto Si(1 1 1) substrates. Black-Right-Pointing-Pointer Three methods RBS, XRR, optical reflectometer were used. Black-Right-Pointing-Pointer The real thickness of each layer was smaller than 50 nm. Black-Right-Pointing-Pointer Ti and TiO{sub 2} film-densities were slightly lower than the corresponding bulk values. -- Abstract: Single-, bi- and tri-layered films of Ti-TiO{sub 2} system were deposited by d.c. pulsed magnetron sputtering from metallic Ti target in an inert Ar or reactive Ar + O{sub 2} atmosphere. The nominal thickness of each layer was 50 nm. The chemical composition and its depth profile were determined by Rutherford backscattering spectroscopy (RBS). Crystallographic structure was analysed by means of X-ray diffraction (XRD) at glancing incidence. X-ray reflectometry (XRR) was used as a complementary method for the film thickness and density evaluation. Modelling of the optical reflectivity spectra of Ti-TiO{sub 2} thin films deposited onto Si(1 1 1) substrates provided an independent estimate of the layer thickness. The combined analysis of RBS, XRR and reflectivity spectra indicated the real thickness of each layer less than 50 nm with TiO{sub 2} film density slightly lower than the corresponding bulk value. Scanning Electron Microscopy (SEM) cross-sectional images revealed the columnar growth of TiO{sub 2} layers. Thickness estimated directly from SEM studies was found to be in a good agreement with the results of RBS, XRR and reflectivity spectra.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Strain rate sensitivity, microstructure variations, and stress-assisted β → α" phase transformation investigation on the mechanical behavior of dual-phase titanium alloys

In this study, the microstructures of three widely used dual-phase titanium alloys: Ti-6Al-4V, Ti-6Al-2Sn-4Zr-2Mo, and Ti-6Al-2Sn-4Zr-6Mo are characterized using backscatter electron imaging and the deformation behaviors in their individual α and β phases are investigated using in situ high-energy X-ray diffraction during uniaxial tension experiments. This is accompanied by calculation of the strain rate sensitivity (SRS) in these alloys, as a function of applied loading. The results of the calculated SRS and the mechanical response (in terms of lattice strains and hardening behaviors) are rationalized based on the local microstructure, composition, and texture of the alloy. A stress-induced β (BCC) to α" (orthorhombic) phase transformation is observed during the in-situ diffraction experiment, which permitted analysis of the lattice strain evolution during the phase transformation. Results from this study provide insights into the relationship between microstructure, composition, applied loading, and the deformation behavior, including effects on loading with time holds. Specifically, the results show that the microstructure, and not necessarily the chemical composition (Mo content), along with the applied loading have a dominant role in the observed SRS variation in titanium alloys. Further, the evolution of the α" (orthorhombic) phase is observed for the first time during deformation of an industrially relevant titanium alloy, Ti-6246.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Molecular beam epitaxy growth and characterization of GePb alloys

Pb based group-IV alloys such as GePb have been gaining interest as a potential alternative for infrared detectors, quantum materials, and high-speed electronic devices. Challenges remain in their growth due to the extremely low solid solubility of Pb in the Ge–Pb system. This paper reports molecular beam epitaxy growth of GePb alloy thin films on Ge(100) substrates. Effusion cells of Ge and Pb are used to control the flux ratio independently. The optimal substrate temperature is found to be near the thermocouple temperature of 300 °C based on the characterization of the grown films using high-resolution x-ray diffraction. A large change in the Ge:Pb beam equivalent pressure ratio from 10:1 to 1:1 results in only a minimal increase of the Pb composition from 0.74% to 2.84% as estimated from Raman spectroscopy and Rutherford backscattering spectrometry. Furthermore, scanning electron microscopy images show a large volume of Pb islands on the surface that form into either long trapezoidal rods or uniform droplets, with increasing Pb flux and growth time the density of Pb islands increased.

36 MATERIALS SCIENCE↗