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At least 1,315 records · Page 73

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DOE OSTI2015

The evolution with strain of the stored energy in different texture components of cold-rolled IF steel revealed by high resolution X-ray diffraction

During the deformation of low carbon steel by cold-rolling, dislocations are created and stored in grains depending on local crystallographic orientation, deformation, and deformation gradient. Orientation dependent dislocation densities have been estimated from the broadening of X-ray diffraction lines measured on a synchrotron beamline. Different cold-rolling levels (from 30% to 95% thickness reduction) have been considered. It is shown that the present measurements are consistent with the hypothesis of the sole consideration of screw dislocations for the analysis of the data. The presented evolutions show that the dislocation density first increases within the α fiber (=(hkl)<110>) and then within the γ fiber (=(111) ). A comparison with EBSD measurements is done and confirms that the storage of dislocations during the deformation process is orientation dependent and that this dependence is correlated to the cold-rolling level. If we assume that this dislocation density acts as a driving force during recrystallization, these observations can explain the fact that the recrystallization mechanisms are generally different after moderate or large strains. - Highlights: • Dislocation densities are assessed by XRD in main texture components of a steel sheet. • Dislocation densities vary with both strain and texture components. • The analysis relies on the sole presence of screw dislocations. • The measured dislocation densities include the contribution of both SSD and GND.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Assessment of firing conditions in old fired-clay bricks: The contribution of X-ray powder diffraction with the Rietveld method and small angle neutron scattering

Full characterization of fired-clay bricks is crucial for the improvement of process variables in manufacturing and, in case of old bricks, for restoration/replacement purposes. To this aim, five bricks produced in a plant in Czech Republic in the past have been investigated with a combination of analytical techniques in order to derive information on the firing process. An additional old brick from another brickyard was also used to study the influence of different raw materials on sample microstructure. The potential of X-ray diffraction with the Rietveld method and small angle neutron scattering technique has been exploited to describe the phase transformations taking place during firing and characterize the brick microstructure. Unit-cell parameter of spinel and amount of hematite are proposed as indicators of the maximum firing temperature, although for the latter, limited to bricks produced from the same raw material. The fractal quality of the surface area of pores obtained from small angle neutron scattering is also suggested as a method to distinguish between bricks produced from different raw clays. - Highlights: • Rietveld method helps in describing microstructure and physical properties of bricks. • XRPD derived cell parameter of spinel is proposed as an indicator of firing temperature. • SANS effectively describes brick micro and nanostructure, including closed porosity. • Fractal quality of pore surface is proposed as ‘fingerprint’ of brick manufacturing.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Cold rolling texture evolution of TiB2 particle reinforced Al-based composites by Neutron Diffraction and EBSD analysis

Highlights: • Texture development of in-situ TiB{sub 2} particle reinforced Al matrix composites after cold rolling were characterized. • The sum of rolling texture volume fractions has been significantly reduced by the weak texture in particle deformation zone. • Recrystallization nuclei with the Cube and Rotated-Cube orientations were observed in the particle deformation zones. • Small TiB{sub 2} particles within Al grains kept the parallel relationship with surrounding matrix during the deformation. - Abstract: Texture development of particle-reinforced metal matrix materials (P-MMCs) has not been understood well, especially the effects of second-phase particles during the deformation. In this work, we have investigated the texture evolution of TiB{sub 2}/Al composites during cold rolling by Neutron Diffraction and EBSD analysis. Two forms of TiB{sub 2} particles influenced the texture evolution in different ways. The particle-clusters aggregated along grain boundaries led to a reduction of texture volume fraction; recrystallization nuclei with weak texture appeared around these particle-clusters. Small non-shearable TiB{sub 2} particles dispersed inside Al matrix contributed to strong Copper texture component at high strains; the individual particles rotated together with Al matrix during the deformation. These revealed effects of particles on the texture development in TiB{sub 2}/Al composites provide a reference for the texture control of P-MMCs.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Direct measurement of the effective properties of an additively manufactured titanium octet truss unit cell using high energy X-ray diffraction

Additively manufactured lattice structures offer a high specific strength-to-density ratio in comparison to conventional, fully dense parts. The small feature size and intricate geometry of lattice structures make it challenging to directly characterize their mechanical properties. This study presents direct measurement of the elastic mechanical properties of an additively manufactured titanium alloy octet truss unit cell. Strut stress and strain were measured using high-energy X-ray diffraction during quasi-static compressive loading. The crystallographic stress-strain relationship was converted into the stress-strain relationship of the octet truss lattice unit cell using the known symmetry of the struts. The sample studied herein was best fit by an orthorhombic linear elastic stress-strain relationship. In conclusion, this technique shows promise for studying additively manufactured lattice structures at length scales not previously reported.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Multicycle flash sintering of cubic Y 2 O 3 -stabilized ZrO 2 : An in situ energy dispersive synchrotron x-ray diffraction study with high temporal resolution

The current induced unit cell volume changes, (111) Bragg peak full width at half maximum (FWHM) and its integrated intensity in 8 % Y 2 O 3 stabilized ZrO 2 (8 %YSZ) solid state electrolyte was monitored during a triple-flash sintering experiment by in situ energy dispersive x-ray diffraction using a polychromatic synchrotron probe (max, photon energy 200 keV) with 2 second temporal resolution. The first spontaneous singularity in the unit cell volume (+0.54 %) was observed at 899 °C under 15 V/mm applied field intensity, which was associated with 13 mA/mm 2 current draw and an increase in density to 97 %. Following anelastic relaxation of the unit cell volume under open circuit conditions, the same applied field was applied twice in a row which resulted in additional induced singularities at 925 °C (+0.48 %) and 944 °C (+0.42 %). A floating baseline, which was above the thermal expansion baseline, was observed from 833 to 969 °C and was attributed to Joule heating. In conclusion, the singularity at 899 °C is associated with a sharp change in (111) FWHM and a 34 % decrease in integrated peak area that was attributed to changes in the distribution of oxygen vacancies and the changes in their concentration as induced by the applied field in the spontaneous transient stage of flash sintering.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Valence Electron Distributions from Sub-Angstrom Convergent Beam Electron Diffraction

Modern aberration-corrected scanning transmission electron microscopes can acquire four-dimensional data sets (“4D STEM”) by recording convergent beam electron diffraction (CBED) patterns, using precisely positioned, sub-angstrom probes. Here, we demonstrate that these patterns can probe the site symmetry, atomic displacements, and valence electron distributions at individual atomic columns. To this end, 4D STEM CBED patterns were acquired from SrTiO 3 single crystals and compared with patterns calculated using scattering potentials derived from density functional theory. Here, we show that an aspherical valence electron charge build-up at the oxygen sites causes intensity asymmetries in the low-angle scattering portion of the patterns. Using strained SrTiO 3 films containing subtle polar displacements within nanometer-sized domains, it is shown that the high-angle scattering portion in each pattern is sensitive to atomic displacements.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Study of strain propagation in laser irradiated silicon crystal by time-resolved diffraction of K-{alpha} x-ray probe of different photon energies

An experimental study on the time resolved x-ray diffraction from laser shocked silicon crystal, carried out using a 10 TW Ti:sapphire laser system, is presented. The characteristic K{sub {alpha}} x-ray line radiation generated by 45 fs laser produced plasmas of two different target materials (iron and copper) is used as the probe, whereas the stretched pulse of sub-nanosecond duration (pump), derived from the same laser, is used to compress the sample. The use of x-ray probe of different photon energies yields information about the strain over a greater crystal depth. The dynamics of the strain propagation is inferred by monitoring the evolution of rocking curve width of the shocked sample at different time delays between the pump and the probe pulse. The shock velocity deduced from these measurements is {approx}10{sup 6} cm/s, consistent with the sound velocity in bulk silicon. The maximum elastic compression observed is 0.4%, indicating a pressure of 0.8 GPa.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Neutron diffraction studies on chemical and magnetic structure of multiferroic PbFe{sub 0.67}W{sub 0.33}O{sub 3}

We report on the single phase synthesis and room temperature structural characterization of PbFe{sub 0.67}W{sub 0.33}O{sub 3} (PFW) multiferroic. The PFW was synthesized by low temperature sintering, Columbite method. Analysis of powder XRD pattern exhibits single phase formation of PFW with no traces of pyrochlore phase. Detailed analysis of room temperature neutron diffraction (ND) reveals cubic phase at room temperature, space group Pm-3m. The ND pattern clearly reveals magnetic Bragg peak at 2θ = 18.51° (Q = 1.36Å{sup −1}). The refinement of magnetic structure reveals G-type antiferromagnetic structure in PFW at room temperature. The dielectric constant and loss tangent decreases with increasing frequency. The room temperature P-E measurements shows a non-linear slim hysteresis, typical nature of relaxor multiferroics, with saturation and remnant polarizations of P{sub s} = 1.50 μC/cm{sup 2} and P{sub r} = 0.40 μC/cm{sup 2}, respectively.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2014

Time-resolved X-ray diffraction studies of laser-induced acoustic wave propagation in bilayer metallic thin crystals

Phonon propagation across the interface of a Cu/Ag(111) bilayer and transient lattice disorder, induced by a femtosecond 267 nm pulse, in Ag(111) crystal have been measured by means of time resolved X-ray diffraction. A “blast” force due to thermal stress induced by suddenly heated electrons is formed within two picoseconds after excitation and its “blast wave” propagation through the interface and Ag (111) crystal was monitored by the shift and broadening of the rocking curve, I vs. ω, as a function of time after excitation. Lattice disorder, contraction and expansion as well as thermal strain formation and wave propagation have also been measured. The experimental data and mechanism proposed are supported by theoretical simulations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2014

Polarity of semipolar wurtzite crystals: X-ray photoelectron diffraction from GaN(101⁻1) and GaN(202⁻1) surfaces

Polarity of semipolar GaN(101⁻1) (101⁻1⁻) and GaN(202⁻1) (202⁻1⁻) surfaces was determined with X-ray photoelectron diffraction (XPD) using a standard MgKα source. The photoelectron emission from N 1s core level measured in the a-plane of the crystals shows significant differences for the two crystal orientations within the polar angle range of 80–100° from the (0001) normal. It was demonstrated that XPD polar plots recorded in the a-plane are similar for each polarity of the GaN(101⁻1) and GaN(202⁻1) crystals if referred to (0001) crystal axes. For polarity determinations of all important GaN(h0h⁻l) semipolar surfaces, the above given polar angle range is suitable.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2014

Mathematical and computational modeling of the diffraction problems by discrete singularities method

The main objective of this study is reduced the boundary-value problems of scattering and diffraction waves on plane-parallel structures to the singular or hypersingular integral equations. For these cases we use a method of the parametric representations of the integral and pseudo-differential operators. Numerical results of the model scattering problems on periodic and boundary gratings and also on the gratings above a flat screen reflector are presented in this paper.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2014

Performance enhancement of thin film silicon solar cells based on distributed Bragg reflector and diffraction grating

The influence of various designing parameters were investigated and explored for high performance solar cells. Single layer grating based solar cell of 50 μm thickness gives maximum efficiency up to 24 % whereas same efficiency is achieved with the use of three bilayers grating based solar cell of 30 μm thickness. Remarkably, bilayer grating based solar cell design not only gives broadband absorption but also enhancement in efficiency with reduced cell thickness requirement. This absorption enhancement is attributed to the high reflection and diffraction from DBR and grating respectively. The obtained short-circuit current were 29.6, 32.9, 34.6 and 36.05 mA/cm{sup 2} of 5, 10, 20 and 30 μm cell thicknesses respectively. These presented designing efforts would be helpful to design and realize new generation of solar cells.

36 MATERIALS SCIENCE↗

DOE OSTI2015

A short note on physical properties to irradiated nuclear fuel by means of X-ray diffraction and neutron scattering techniques

For nuclear reactor applications, understanding the evolution of the fuel materials microstructure during irradiation are of great importance. This paper reviews the physical properties of irradiated nuclear fuel analysis which are considered to be of most importance in determining the performance behavior of fuel. X-rays diffraction was recognize as important tool to investigate the phase identification while neutron scattering analyses the interaction between uranium and other materials and also investigation of the defect structure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

Electron backscatter diffraction analysis of gold nanoparticles on Y{sub 1}Ba{sub 2}Cu{sub 3}O{sub 7−δ}

It has been shown recently that the incorporation of gold nanoparticles into Y{sub 1}Ba{sub 2}Cu{sub 3}O{sub 7−δ} enhances the superconducting properties of this material in a significant way. Previous XRD and TEM investigations suggest different crystallographic relations of the gold nanoparticles with respect to the epitaxial Y{sub 1}Ba{sub 2}Cu{sub 3}O{sub 7−δ}. Here, detailed investigations of the crystal orientations for a large ensemble of gold nanoparticles with electron backscatter diffraction are reported. The average size of the gold nanoparticles is in the range of 60 nm–80 nm. We identified five different types of heteroepitaxial relationships between the gold nanoparticles and the superconductor film, resulting in complex pole figures. The observed different types of crystallographic orientations are discussed based on good lattice matching and the formation of low energy interfaces.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2015

Refractive-index determination of solids from first- and second-order critical diffraction angles of periodic surface patterns

We present two approaches for measuring the refractive index of transparent solids in the visible spectral range based on diffraction gratings. Both require a small spot with a periodic pattern on the surface of the solid, collimated monochromatic light, and a rotation stage. We demonstrate the methods on a polydimethylsiloxane film (Sylgard{sup ®} 184) and compare our data to those obtained with a standard Abbe refractometer at several wavelengths between 489 and 688 nm. The results of our approaches show good agreement with the refractometer data. Possible error sources are analyzed and discussed in detail; they include mainly the linewidth of the laser and/or the angular resolution of the rotation stage. With narrow-band light sources, an angular accuracy of ±0.025{sup ∘} results in an error of the refractive index of typically ±5 ⋅ 10{sup −4}. Information on the sample thickness is not required.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Optical study of a spectrum splitting solar concentrator based on a combination of a diffraction grating and a Fresnel lens

This paper presents recent improvements of our new solar concentrator design for space application. The concentrator is based on a combination of a diffraction grating (blazed or lamellar) coupled with a Fresnel lens. Thanks to this diffractive/refractive combination, this optical element splits spatially and spectrally the light and focus approximately respectively visible light and IR light onto electrically independent specific cells. It avoid the use of MJs cells and then also their limitations like current matching and lattice matching conditions, leading theoretically to a more tolerant system. The concept is reminded, with recent optimizations, ideal and more realistic results, and the description of an experimental realization highlighting the feasibility of the concept and the closeness of theoretical and experimental results.

14 SOLAR ENERGY↗

DOE OSTI2016

Two-dimensional groove density measurement for gratings by diffraction method

A grating groove density measuring system based on diffraction method has been developed to measure the two-dimensional groove density variations of the VLS gratings at NSRL. The measuring system can provide not only the basic data of the two-dimensional groove density variations for evaluating the imaging properties of grating, but also an important tool for improving the grating manufacturing technology. A commercially available concave grating with a curvature radius of 750 mm was measured to test the accuracy of the measuring system. Results show that the system has a measuring accuracy (ΔN/N) of about 5 × 10{sup −5}. Then the groove density variation parameters of the 1200 lines/mm VLS plane grating used in NSRL is measured by the system. The groove curvature of the VLS plane grating has been observed.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2020

Photodissociation of aqueous I3− observed with liquid-phase ultrafast mega-electron-volt electron diffraction

Developing femtosecond resolution methods for directly observing structural dynamics is critical to understanding complex photochemical reaction mechanisms in solution. We have used two recent developments, ultrafast mega-electron-volt electron sources and vacuum compatible sub-micron thick liquid sheet jets, to enable liquid-phase ultrafast electron diffraction (LUED). We have demonstrated the viability of LUED by investigating the photodissociation of tri-iodide initiated with a 400 nm laser pulse. This has enabled the average speed of the bond expansion to be measured during the first 750 fs of dissociation and the geminate recombination to be directly captured on the picosecond time scale.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗