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At least 847 records · Page 47

Improved Diffraction Efficiency of Polarization-Sensitive Azobenzene-Containing Copolymers in an Electric Field

Recording media for polarization holography based on new azobenzene-containing monomers with octylmethacrylate are created. Their electrophysical and information properties are investigated. Improvement of the diffraction efficiency of holograms in these media in an external electric field formed by charging the free surface of the polymer film in a corona discharge is demonstrated. The diffraction efficiency is improved more in the copolymer, in which the azobenzene fragments possess larger dipole moments.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Boron Doping on High-Resolution X-Ray Diffraction Metrology

The effect of boron (B) doping on high-resolution X-ray diffraction (HXRD) metrology has been investigated. Twelve samples of Si{sub 1–x}Ge{sub x} films were epitaxially grown on Si (100) substrates with different thicknesses, germanium (Ge) concentrations and with/without B dopants. Secondary ion mass spectroscopy (SIMS) and HXRD were employed for measurements of B doping, Ge concentration, strain, and thickness of the layers. The SIMS results show the absence of B in two samples while the rest of the samples have B doping in the range of 8.40 × 10{sup 18}–8.7 × 10{sup 20} atoms/cm{sup 3} with Ge concentration of 13.3–55.2 at.%. The HXRD measurements indicate the layers thickness of 7.07–108.13 nm along with Ge concentration of 12.82–49.09 at.%. The difference in the Ge concentration measured by SIMS and HXRD was found to deend on B doping. For the undoped samples, the difference is ~0.5 at.% and increases with B doping but with no linear proportionality. The difference in the Ge concentration was 7.11 at.% for the highly B-doped (8.7 × 10{sup 20} atoms/cm{sup 3}) sample. The B doping influences the Si{sub 1–x}Ge{sub x} structure, causing a change in the lattice parameter and producing tensile strains shifting Si{sub 1–x}Ge{sub x} peaks towards Si (100) substrate peaks in the HXRD diffraction patterns. As a result, Vegard’s law is no longer effective and makes a high impact on the HXRD measurement. The comparison between symmetric (004) and asymmetric (+113, +224) reciprocal space mappings (RSM) showed a slight difference in Ge concentration between the undoped and lower B-doped samples. However, there is a change of 0.21 at.% observed for the highly doped Si{sub 1–x}Ge{sub x} samples. RSM’s (+113) demonstrate the small SiGe peak broadening as B doping increases, which indicates a minor crystal distortion.

36 MATERIALS SCIENCE↗

Using in operando diffraction to relate lattice strain with degradation mechanism in a NMC battery

Crystallographic structural changes in a commercial 5 Ah prismatic graphite–NMC battery were investigated during its operation using energy-dispersive X-ray diffraction. The characteristic diffraction peaks for the anode and cathode were identified, and their peak positions were linked to the charge–discharge cycle of the battery. Here, the edge of the negative terminal of battery was shown to undergo irregular cycling behavior. Stresses developed at the battery layer interfaces were proposed to be the source for this deterioration, which limits the lifetime of the battery. The effect of pulse discharge on strain in cathode has also been studied.

36 MATERIALS SCIENCE↗

Magnetism in Solid Oxygen Studied by High-Pressure Neutron Diffraction

This article reviews progress achieved over the last ~ 15 years in our understanding of magnetism in solid oxygen under high pressure with a particular emphasis on the contribution of neutron diffraction in the multi-GPa range. The paper highlights the unexpected complexity of magnetic structures in the δ phase at 5–8 GPa, presents data on the pressure dependence of diffuse scattering in β-O{sub 2} and discusses potential magnetism in ε-O{sub 2}. High-resolution diffraction data of all three solid phases at ambient pressure are presented.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Interpretation of Indications Generated by Small Welding Discontinuities in Ultrasonic Time of Flight Diffraction Technique

The article presents results of research on non-destructive ultrasonic time of flight diffraction technique TOFD and metallographic examinations of selected cross-sections of a MAG welded joint. The main objective was to compare the results of TOFD and metallographic examination at the locations where a large number of point-like indications, located on specific depths, have been detected on TOFD images and analyse the impact of this type of indication on results of a welded joint evaluation. Considered, that the indications have not exhibited separations between upper and lower diffraction signals, because of their small heights, measuring of height of indications in those cases was impossible. In all cases, the occurrence of discontinuities of 0.16–0.78 mm in height, in locations indicated by TOFD has been confirmed.

42 ENGINEERING↗

Crystal Structure of (Lu{sub 1−x}Ca{sub x})Ba{sub 2}Cu{sub 3}O{sub 7−z} (x = 0, 0.2) Superconducting Compounds Studied by Neutron Powder Diffraction

The crystalline structures of two polycrystalline samples of (Lu{sub 1−x}Ca{sub x})Ba{sub 2}Cu{sub 3}O{sub 7−z} with x = 0 (pure sample) and x = 0.2 (Ca-doped sample) have been analyzed by using neutron powder diffraction techniques to address the structural mechanisms associated with changes in superconducting behavior induced by Ca doping. The pure and Ca-doped samples exhibit superconductivity around 87 and 32 K, respectively. The room-temperature thermoelectric power measurements indicate that both the x = 0 and 0.2 samples are in overdoped state. The Rietveld refinements of the neutron diffraction data collected at room temperature for the pure and Ca-doped samples show that the higher level of oxygen vacancies is located on both the CuO{sub 2} planes and the apical oxygen sites for the pure sample compared to those of the Ca-doped sample. The present results suggest that the decrease in T{sub c} observed in the Ca-doped sample is mainly caused by the hole overdoping effect rather than by oxygen vacancies in the CuO{sub 2} planes.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Scattering Amplitudes in a Neighborhood of Limit Rays in Short-Wave Diffraction by Elongated Bodies of Revolution

In the paper, diffraction problems of a plane wave by smooth, convex, and elongated bodies of revolution are considered within the framework of short-wave approximation (axially symmetric cases). The scattering amplitudes are calculated in the direction of limit rays, and the influence of the elongation of the scatterers on the amplitudes behavior is investigated. Mathematical techniques of our approach are based on the Green’s formulas in the exterior of the scatterers and numerical calculations of the wave field current in the boundary layers in the vicinity of the light-shadow zone. It is established that the elongation of axially symmetric bodies relatively weakly affects the scattering amplitudes of the short-wave asymptotics. The main contribution to the amplitudes is made by the solution of the 2D diffraction problem by a convex, smooth curve in the cross section of the scatterers by a plane containing the rotation axis.

97 MATHEMATICS AND COMPUTING↗

Physical Interpretation of Strict Solutions of Diffraction Problems by Heuristic Relations

We propose a new approach to construct heuristic relations describing solutions of diffraction problems. Those relations are based on physical principles and allow one to interpret mathematically strict solutions. Since the heuristic relations possess high performance and accuracy, they can also be used along with any strict approach or experimental results for a significant improvement of efficiency of solutions of practical problems related to applications of the diffraction theory.

97 MATHEMATICS AND COMPUTING↗

Generation of spiraling Bessel beams from dark/antidark Gaussian beams diffracted by a curved fork-shaped hologram

In this paper, we present a theoretical study on the generation of spiraling Bessel beams by illuminating a curved fork-shaped hologram (CFH) by spatially coherent dark/antidark Gaussian beams. The amplitude expression of the generated spiraling Bessel beam is obtained by using the framework of the Fresnel diffraction approach and by means of the stationary phase method. Numerical calculations show that upon propagating, the longitudinal intensity of the generated field reaches a threshold maximum value at a distance z{sub max}. It is demonstrated that z{sub max} increases with the increasing of the topological charge p and the order m. The result corresponding to the incident Gaussian beam diffracted by CFH is obtained as a particular case of this study.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Holographic Formation of Diffraction Elements for Transformation of Light Beams in Liquid Crystal – Photopolymer Compositions

A theoretical model of holographic formation of diffractive optical elements for transformation of light beam field into Bessel-like fields in liquid crystal – photopolymer (LC–PPM) composite materials with a dyesensitizer is developed. Results of numerical modeling of kinetics ofvariation of the refractive index of a material in the process of formation with different relationships between the photopolymerization rates and diffusion processes are presented. Based on the results of numerical simulation, it is demonstrated that when the photopolarization process dominates, the diffractive element being formed is distorted. This leads to a change in the light field distribution at its output and consequently, to ineffective transformation of the reading beam. Thus, the necessity of optimizing of the recording conditions and of the prepolymeric composition to increase the transformation efficiency of light beam fields is demonstrated.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Oil-Pressure Based Apparatus for In-Situ High-Energy Synchrotron X-Ray Diffraction Studies During Biaxial Deformation

Background: Understanding biaxial loading response at the microstructural level is crucial in helping better design sheet manufacturing processes and calibrate/validate material deformation models. Objective: The objective of this work was to develop a low-cost testing apparatus to probe, with sufficient spatial resolution, the micro-mechanical response of a sheet material in-situ under biaxial loading conditions. Methods: The testing apparatus fabricated as a part of this study operates in a similar fashion to a standard bulge test and uses oil pressure to generate biaxial loading conditions. This biaxial testing apparatus was operated within a synchrotron beamline to characterize the mechanical response of a flash-processed steel sheet using in-situ high-energy X-ray diffraction (XRD) measurements. Further, the GSAS-II package was utilized to develop a workflow for the analysis of the large volume of diffraction data acquired. The workflow was then used to extract the peak position, width, and integrated intensity of the XRD peaks corresponding to the major body-centered cubic phase. Results: The equi-biaxial nature of the loading in the measured area was independently corroborated using experimental (XRD) and simulation (finite element analysis) methods. Furthermore, we discuss the evolution of elastic strain in the major body-centered cubic phase as a function of applied oil pressure and location on the steel sheet. Conclusions: A key advantage of the biaxial apparatus fabricated in this synchrotron study is demonstrated using the results obtained for the flash-processed steel sheet – i.e., mapping the lattice plane-dependent response to biaxial loading for a relatively large sample area in a spatially resolved manner.

36 MATERIALS SCIENCE↗

In Situ X-Ray Diffraction Analysis of Face-Centered Cubic Metals Deformed at Room and Cryogenic Temperatures

The present study concerns the cryogenic processing of metals with simultaneous analysis of x-ray diffraction in a synchrotron ring. The mechanical properties improvement related to cryogenic processing of metals is attributed to the partial suppression of dynamic recovery. Thus, commercially pure metals with different stacking fault energies (silver, copper and aluminum) were deformed by uniaxial tensile tests and characterized by in situ x-ray diffraction, at room (293 K) and cryogenic (77 K) temperatures. The cryogenic processing allows a simultaneous improvement in ductility and strength for silver and copper and an improvement in strength for aluminum. This difference in mechanical properties was investigated by means of variations in crystallite size, microstrain and also the amount and size of dimples on the fracture surface. The microstructural refinement at cryogenic temperatures shows a tendency related to the stacking fault energies.

36 MATERIALS SCIENCE↗

Microscale Observation via High-Speed X-ray Diffraction of Alloy 718 During In Situ Laser Melting

The laser melting process is accompanied by rapid evolution in temperature, phase, structure, and strain because of its high heating and cooling rates. In this study, the evolution of grains within a thin solid plate of Ni alloy 718 during laser processing was probed with in situ high-energy x-ray diffraction experiments. The high temporal and spatial resolution available in the measurement allowed us to study the rapid evolution of the melted region beneath the surface of the sample. The characterization of the evolution of secondary phases, i.e., Laves and carbide, was captured despite the weak diffracted peaks caused by small volume fractions. Thermal history was estimated based on changes in the lattice spacing from the thermal contraction upon cooling. In conclusion, the temporal variation in 2θ with azimuthal direction revealed the evolution in anisotropy of lattice spacing and thus of the mechanical state during laser processing.

36 MATERIALS SCIENCE↗

Unraveling cyclic deformation mechanisms of a rolled magnesium alloy using in situ neutron diffraction

In the current study, the deformation mechanisms of a rolled magnesium alloy were investigated under cyclic loading using real-time in situ neutron diffraction under a continuous-loading condition. The relationship between the macroscopic cyclic deformation behavior and the microscopic response at the grain level was established. The neutron diffraction results indicate that more and more grains are involved in the twinning and detwinning deformation process with the increase of fatigue cycles. The residual twins appear in the early fatigue life, which is responsible for the cyclic hardening behavior. The asymmetric shape of the hysteresis loop is attributed to the early exhaustion of the detwinning process during compression, which leads to the activation of dislocation slips and rapid strain-hardening. The critical resolved shear stress for the activation of tensile twinning closely depends on the residual strain developed during cyclic loading. In the cycle before the sample fractured, the dislocation slips became active in tension, although the sample was not fully twinned. The increased dislocation density leads to the rise of the stress concentration at weak spots, which is believed to be the main reason for the fatigue failure. Furthermore, the deformation history greatly influences the deformation mechanisms of hexagonal-close-packed-structured magnesium alloy during cyclic loading.

36 MATERIALS SCIENCE↗

In situ high-energy X-ray diffraction study of tensile deformation of neutron-irradiated polycrystalline Fe-9%Cr alloy

The effect of neutron irradiation on tensile deformation of a Fe-9wt.%Cr alloy was investigated using in situ high-energy synchrotron X-ray diffraction during room-temperature uniaxial tensile tests. New insights into the deformation mechanisms were obtained through the measurements of lattice strain evolution and the analysis of diffraction peak broadening using the modified Williamson-Hall method. Two neutron-irradiated specimens, one irradiated at 300 °C to 0.01 dpa and the other at 450 °C to 0.01dpa, were tested along with an unirradiated specimen. The macroscopic stress–strain curves of the irradiated specimens showed increased strength, reduced ductility and work-hardening exponent compared to the unirradiated specimen. The evolutions of the lattice strain, the dislocation density and the coherent scattering domain size in the deformation process revealed different roles of the submicroscopic defects in the 300°C/0.01 dpa specimen and the TEM-visible nanometer-sized dislocation loops in the 450°C/0.01 dpa specimen: submicroscopic defects extended the linear work hardening stage (stage II) to a higher strain, while irradiation-induced dislocation loops were more effective in dislocation pinning. Lastly, while the work hardening rate of stage II was unaffected by irradiation, significant dynamic recovery in stage III in the irradiated specimens led to the early onset of necking without stage IV as observed in the unirradiated specimen.

36 MATERIALS SCIENCE↗

In situ high energy X-ray diffraction measurement of strain and dislocation density ahead of crack tips grown in hydrogen

The deformation fields near fatigue crack tips grown in hydrogen and in air were measured using high-energy x-ray diffraction. A larger magnitude of elastic strain was observed in the hydrogen case compared to the air case. The magnitude of elastic strain was quantified through an effective crack tip stress intensity factor. The dislocation profile ahead of the crack was probed via x-ray line broadening and electron back-scatter diffraction was used to assess the crack path (intergranular vs. transgranular). Ahead of the crack tip grown in hydrogen, an order of magnitude lower dislocation density, compared to a baseline density far from the crack, was observed. This decrease in dislocation density was not observed in the air case. These differences are discussed in terms of two leading hydrogen embrittlement mechanisms, Hydrogen Enhanced Localized Plasticity (HELP) and Hydrogen Enhanced Decohesion (HEDE). We have observed a decrease in transgranular cohesion (transgranular HEDE), as well as an increase in intergranular fracture. The measurements of dislocation activity support a model of a decrease in intergranular cohesion (intergranular HEDE) which is likely facilitated by the HELP mechanism. Here, this suggests that the increase in fatigue crack growth rate is due to a sum of the two effects of hydrogen, in which the crack grows faster in the transgranular fracture mode and faster due to an increase in a new mode of intergranular fracture. Published by Elsevier Ltd on behalf of Acta Materialia Inc.

36 MATERIALS SCIENCE↗

Melting and solidification dynamics during laser melting of reaction-based metal matrix composites uncovered by in-situ synchrotron X-ray diffraction

Laser additive manufacturing (AM) of reaction-based metal matrix composites (MMCs) involves highly complex and non-equilibrium material transformation behavior, including melting, dissolution, precipitation, and solidification. Yet, the dynamics and interplay of these phase transformation processes remain poorly understood, posing substantial challenges in identifying the microstructure formation mechanism, and predicting and controlling the microstructure in the printed parts. Here, in this study, we performed the in-situ X-ray diffraction experiment to characterize the phase evolution dynamics of the 316L + 10 vol.%TiC system during laser melting, which provides direct and quantitative insights of the complex phase reaction and evolution dynamics under rapid heating and cooling conditions relevant to additive manufacturing of reaction-based MMCs. Further in-depth thermodynamic and kinetic calculations revealed that most of the phase evolution behavior observed in the in-situ X-ray diffraction experiment cannot be solely explained by widely used equilibrium thermodynamic models, and diffusion-controlled nonequilibrium dissolution and precipitation kinetics must be considered to elucidate the complex phase evolution behavior, including incomplete TiC dissolution, and three-step TiC precipitation. The three distinct types of precipitates generate unique hierarchical TiC micro- and nanostructures, which enhances the yield strength from 513 MPa to 877 MPa by 71 %, tensile strength from 628 MPa to 1054 MPa by 68 %, and Young's modulus from 193 GPa to 221 GPa by 14 %. The findings of our research provide the knowledge foundation for the design of unique microstructures and advanced MMC materials through laser AM.

36 MATERIALS SCIENCE↗

Characterization of morphology and hydration products of high-volume fly ash paste by monochromatic scanning x-ray micro-diffraction (μ-SXRD)

The present study focuses on identification and micro-structural characterization of the hydration products formed in high-volume fly ash (HVFA)/portland cement (PC) systems using monochromatic scanning x-ray micro-diffraction (μ-SXRD) and SEM-EDS. Pastes with up to 80% fly ash replacement were studied. Phase maps for HVFA samples using μ-SXRD patterns prove that μ-SXRD is an effective method to identify and visualize the distribution of phases in the matrix. μ-SXRD and SEM-EDS analysis shows that the C-S-H formed in HVFA system containing 50% or more of fly ash has a similar structure as C-S-H(I) with comparatively lower Ca/Si ratio than the one produced in PC system. Moreover, coexistence of C-S-H(I) and strätlingite is observed in the system containing 80% of fly ash, confirming that the amount of alumina and silicate phases provided by the fly ash is a major factor for the formation of C-S-H(I) and strätlingite in HVFA system. - Highlights: • High-volume fly ash (HVFA) paste was studied by scanning x-ray micro-diffraction. • Coexistence of C-S-H(I) and strätlingite in the HVFA system is clearly shown. • The distribution of minor phases in the HVFA system is shown. • Differences between inner and outer products of fly ash are observed by SEM-EDS.

36 MATERIALS SCIENCE↗