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iCHORD-SI combination as an alternative to EDS-EBSD coupling for the characterization of γ-γ′ nickel-based superalloy microstructures
Highlights: • A new method to get orientation maps discriminating the gamma and gamma’ phases of Ni superalloys is described. • The method combines the iCHORD technique with secondary ion imaging. • The new method resolves precipitates down to 150 nm within a reasonable acquisition time. - Abstract: Because they exhibit very similar diffraction patterns, the γ and γ′ phases of nickel-based superalloys cannot be distinguished by the conventional EBSD technique alone. This paper presents an original method which discriminates those phases on an orientation map by exploiting their chemical differences. Performed with a Focused Ion Beam (FIB) microscope, the method is the combination of the ion CHanneling ORientation Determination technique (iCHORD) – recently developed by Langlois et al. [1] – with the chemical information obtained from Secondary Ion (SI) images. The performances of the method are compared to the EDS-EBSD coupling which also discriminates phases based on their chemical compositions. Applied filters, angular resolution, spatial resolution of the phase discrimination and acquisition time are discussed. It results that the iCHORD–SI combination offers an orientation map with an angular resolution slightly decreased compared to that of the EBSD technique, but with a good phase resolution (down to 150 nm) and within a reasonable acquisition time. Thus, the iCHORD–SI combination appears to be an interesting method for the crystallographic systems where phases are difficult to discriminate by the EBSD technique alone but present a significant chemical contrast.
NMR study of Ni 50+x Ti 50-x strain glasses
Here, we studied Ni 50+x Ti 50-x with compositions up to x = 2, performing 47 Ti and 49 Ti nuclear magnetic resonance (NMR) measurements from 4 to 400 K. For large x in this system, a strain glass appears in which frozen ferroelastic nanodomains replace the displacive martensite structural transition. Here, we demonstrate that NMR can provide an extremely effective probe of the strain-glass freezing process, with large changes in NMR line shape due to the effects of random strains which become motionally narrowed at high temperatures. At the same time with high-resolution x-ray diffraction we confirm the lack of structural changes in x ≥ 1.2 samples, while we show that there is little change in the electronic behavior across the strain-glass freezing temperature. NMR spin-lattice relaxation time (T 1 ) measurements provide a further measure of the dynamics of the freezing process, and indicate a predominantly thermally activated behavior both above and below the strain-glass freezing temperature. We show that the strain-glass results are consistent with a very small density of critically divergent domains undergoing a Vogel-Fulcher-type freezing process, coexisting with domains exhibiting faster dynamics and stronger pinning.
Creating Ruddlesden-Popper phases by hybrid molecular beam epitaxy
The synthesis of a 50 unit cell thick n = 4 Sr{sub n+1}Ti{sub n}O{sub 3n+1} (Sr{sub 5}Ti{sub 4}O{sub 13}) Ruddlesden-Popper (RP) phase film is demonstrated by sequentially depositing SrO and TiO{sub 2} layers in an alternating fashion using hybrid molecular beam epitaxy (MBE), where Ti was supplied using titanium tetraisopropoxide (TTIP). A detailed calibration procedure is outlined for determining the shuttering times to deposit SrO and TiO{sub 2} layers with precise monolayer doses using in-situ reflection high energy electron diffraction (RHEED) as feedback. Using optimized Sr and TTIP shuttering times, a fully automated growth of the n = 4 RP phase was carried out over a period of >4.5 h. Very stable RHEED intensity oscillations were observed over the entire growth period. The structural characterization by X-ray diffraction and high resolution transmission electron microscopy revealed that a constant periodicity of four SrTiO{sub 3} perovskite unit cell blocks separating the double SrO rocksalt layer was maintained throughout the entire film thickness with a very little amount of planar faults oriented perpendicular to the growth front direction. These results illustrate that hybrid MBE is capable of layer-by-layer growth with atomic level precision and excellent flux stability.
Correlated Single-Crystal Electronic Absorption Spectroscopy and X-ray Crystallography at NSLS Beamline X26-C
The research philosophy and new capabilities installed at NSLS beamline X26-C to support electronic absorption and Raman spectroscopies coupled with X-ray diffraction are reviewed. This beamline is dedicated full time to multidisciplinary studies with goals that include revealing the relationship between the electronic and atomic structures in macromolecules. The beamline instrumentation has been fully integrated such that optical absorption spectra and X-ray diffraction images are interlaced. Therefore, optical changes induced by X-ray exposure can be correlated with X-ray diffraction data collection. The installation of Raman spectroscopy into the beamline is also briefly reviewed. Data are now routinely generated almost simultaneously from three complementary types of experiments from the same sample. The beamline is available now to the NSLS general user population.
Annealing effect on the particle size and chemical composition of activated carbon obtained from vacuum furnace of teak sawdust
Activated carbon was produced from sawdust by using physical method in a high temperature vacuum furnace without additional chemical. Fast pyrolysis process was carried out prior in fluidized a bed furnace to produce char before activation process. Experiments were conducted to investigate the influence of various process parameters such as particle size, activation temperature and activation time on the quality of the activated carbon. In addition, the chemical composition studies were done by using x-ray fluorescence (XRF) spectroscopy. The crystallite sizes were calculated by using Scherer equation based on x-ray diffraction (XRD) spectroscopy data. The pyrolysis temperature and time were varied from 600°C to 900°C and from 3 hours to 6 hours, respectively. The particle size of activated carbon was increase with increasing temperature. The composition and crystallite size of the prepared activated carbon was compared with the non-activated carbon. The results indicated that the teak sawdust carbon could be employed as a low cost alternative to produce commercial activated carbon.
Electro-Optic Time-to-Space Converter for Optical Detector Jitter Mitigation
A common problem in optical detection is determining the arrival time of a weak optical pulse that may comprise only one to a few photons. Currently, this problem is solved by using a photodetector to convert the optical signal to an electronic signal. The timing of the electrical signal is used to infer the timing of the optical pulse, but error is introduced by random delay between the absorption of the optical pulse and the creation of the electrical one. To eliminate this error, a time-to-space converter separates a sequence of optical pulses and sends them to different photodetectors, depending on their arrival time. The random delay, called jitter, is at least 20 picoseconds for the best detectors capable of detecting the weakest optical pulses, a single photon, and can be as great as 500 picoseconds. This limits the resolution with which the timing of the optical pulse can be measured. The time-to-space converter overcomes this limitation. Generally, the time-to-space converter imparts a time-dependent momentum shift to the incoming optical pulses, followed by an optical system that separates photons of different momenta. As an example, an electro-optic phase modulator can be used to apply longitudinal momentum changes (frequency changes) that vary in time, followed by an optical spectrometer (such as a diffraction grating), which separates photons with different momenta into different paths and directs them to impinge upon an array of photodetectors. The pulse arrival time is then inferred by measuring which photodetector receives the pulse. The use of a time-to-space converter mitigates detector jitter and improves the resolution with which the timing of an optical pulse is determined. Also, the application of the converter enables the demodulation of a pulse position modulated signal (PPM) at higher bandwidths than using previous photodetector technology. This allows the creation of a receiver for a communication system with high bandwidth and high bits/photon efficiency.
Design and construction of a compact, high-repetition-rate ultrafast electron diffraction instrument
We present the design and performance of a compact ultrafast electron diffraction instrument. The diffractometer provides a means of examining time-resolved ultrafast dynamical properties of solids. The system’s utilization is discussed in terms of instrument parameters and diffraction data from selected condensed matter samples. Here, the difractometer’s performance is highlighted in terms of detection sensitivity, instrumental temporal resolution, and the electron beam transverse coherence length. Following specific details of the construction, we present a practical discussion of parameters such as repetition rate and provide advice on general construction approaches for laboratory-based, keV ultrafast electron diffractometers. In addition, design guidance for constructing a compact electron gun source that is well-suited for studying diffraction from hard condensed matter is given. A unique data acquisition scheme, utilizing high laser repetition rates, is presented.
Femtosecond diffraction dynamics of laser-induced periodic surface structures on fused silica
The formation of laser-induced periodic surface structures (LIPSS) on fused silica upon irradiation with linearly polarized fs-laser pulses (50 fs pulse duration, 800 nm center wavelength) is studied experimentally using a transillumination femtosecond time-resolved (0.1 ps-1 ns) pump-probe diffraction approach. This allows to reveal the generation dynamics of near-wavelength-sized LIPSS showing a transient diffraction at specific spatial frequencies even before a corresponding permanent surface relief was observed. The results confirm that the ultrafast energy deposition to the materials surface plays a key role and triggers subsequent physical mechanisms such as carrier scattering into self-trapped excitons.
Accurate quantification of lattice temperature dynamics from ultrafast electron diffraction of single-crystal films using dynamical scattering simulations
In ultrafast electron diffraction (UED) experiments, accurate retrieval of time-resolved structural parameters, such as atomic coordinates and thermal displacement parameters, requires an accurate scattering model. Unfortunately, kinematical models are often inaccurate even for relativistic electron probes, especially for dense, oriented single crystals where strong channeling and multiple scattering effects are present. This article introduces and demonstrates dynamical scattering models tailored for quantitative analysis of UED experiments performed on single-crystal films. As a case study, we examine ultrafast laser heating of single-crystal gold films. Comparison of kinematical and dynamical models reveals the strong effects of dynamical scattering within nm-scale films and their dependence on sample topography and probe kinetic energy. Applying to UED experiments on an 11 nm thick film using 750 keV electron probe pulses, the dynamical models provide a tenfold improvement over a comparable kinematical model in matching the measured UED patterns. Also, the retrieved lattice temperature rise is in very good agreement with predictions based on previously measured optical constants of gold, whereas fitting the Debye–Waller factor retrieves values that are more than three times lower. Altogether, these results show the importance of a dynamical scattering theory for quantitative analysis of UED and demonstrate models that can be practically applied to single-crystal materials and heterostructures.
X-Ray Performance of Critical-angle Transmission Grating Prototypes for the Arcus Mission
Arcus is a proposed Explorer Class soft X-ray grating spectrometer. It aims to explore cosmic feedback by mapping hot gases within and between galaxies and galaxy clusters and characterizing jets and winds from supermassive black holes and to investigate the dynamics of protoplanetary disks and stellar accretion. Arcus features 12 m focal-length grazing-incidence silicon pore optics (SPO) developed for the Athena mission. Critical-angle transmission (CAT) gratings efficiently disperse high diffraction orders onto CCDs. We report new and improved X-ray performance results for Arcus-like CAT gratings, including a record resolving power for two coaligned CAT gratings. Multiple Arcus prototype grating facets were illuminated by an SPO at the PANTER facility. The facets consist of 32 × 32.5 mm 2 patterned silicon membranes, bonded to metal frames. The bonding angle is adjusted according to the measured average tilt angle of the grating bars in the membrane. Two simultaneously illuminated facets show a minor broadening of the Al-K α doublet in the 18th and 21st orders with the best-fit record effective resolving power of ${R}_{G}\approx {1.3}_{-0.5}^{+\infty }\times {10}^{4}$ (3σ), about three to four times the Arcus requirement. We measured the diffraction efficiency of quasi-fully illuminated gratings at O-K wavelengths in orders 4–7 in an Arcus-like configuration and compare results with synchrotron spot measurements. After corrections for geometrical effects and bremsstrahlung continuum, we find agreement between full and spot illumination at the two different facilities, as well as with the models used for Arcus effective area predictions. We find that these flight-like gratings meet the diffraction efficiency and greatly exceed the resolving power Arcus requires.
Note: An X-ray powder diffractometer with a wide scattering-angle range of 72° using asymmetrically positioned one-dimensional detectors
An X-ray powder diffractometer has been developed for a time-resolved measurement without the requirement of a scattering angle (2θ) scan. Six one-dimensional detector modules are asymmetrically arranged in a vertical line at a designed distance of 286.5 mm. A detector module actually covers a diffraction angle of about 12° with an angular resolution of 0.01°. A diffracted intensity pattern is simultaneously recorded in a 2θ angular range from 1.63° to 74.37° in a “one shot” measurement. We tested the performance of the diffractometer with reference CeO{sub 2} powders and demonstrated diffraction measurements from an operating lithium-air battery.
Development of the charge exchange recombination spectroscopy and the beam emission spectroscopy on the EAST tokamak
Charge eXchange Recombination Spectroscopy (CXRS) and Beam Emission Spectroscopy (BES) diagnostics based on a heating neutral beam have recently been installed on EAST to provide local measurements of ion temperature, velocity, and density. The system design features common light collection optics for CXRS and BES, background channels for the toroidal views, multi-chord viewing sightlines, and high throughput lens-based spectrometers with good signal to noise ratio for high time resolution measurements. Additionally, two spectrometers each has a tunable grating to observe any wavelength of interest are used for the CXRS and one utilizes a fixed-wavelength grating to achieve higher diffraction efficiency for the BES system. A real-time wavelength correction is implemented to achieve a high-accuracy wavelength calibration. Alignment and calibration are performed. Initial performance test results are presented.
Time-stretch microscopy based on time-wavelength sequence reconstruction from wideband incoherent source
Time-stretch microscopy has emerged as an ultrafast optical imaging concept offering the unprecedented combination of the imaging speed and sensitivity. However, dedicated wideband and coherence optical pulse source with high shot-to-shot stability has been mandated for time-wavelength mapping—the enabling process for ultrahigh speed wavelength-encoded image retrieval. From the practical point of view, exploiting methods to relax the stringent requirements (e.g., temporal stability and coherence) for the source of time-stretch microscopy is thus of great value. In this paper, we demonstrated time-stretch microscopy by reconstructing the time-wavelength mapping sequence from a wideband incoherent source. Utilizing the time-lens focusing mechanism mediated by a narrow-band pulse source, this approach allows generation of a wideband incoherent source, with the spectral efficiency enhanced by a factor of 18. As a proof-of-principle demonstration, time-stretch imaging with the scan rate as high as MHz and diffraction-limited resolution is achieved based on the wideband incoherent source. We note that the concept of time-wavelength sequence reconstruction from wideband incoherent source can also be generalized to any high-speed optical real-time measurements, where wavelength is acted as the information carrier.
Unveiling the spatial distribution of molecular coherences at conical intersections by covariance X-ray diffraction signals
Significance Monitoring the real-space motion of the electrons directly involved in ultrafast molecular dynamics is a challenging goal, hindered by the strong contributions of the remaining inactive electrons. Molecular quantum coherences can provide a direct window into elementary electronic dynamics, but they could not be separately imaged so far. Here, we demonstrate a time- and frequency-resolved X-ray diffraction technique, which can employ existing stochastic X-ray pulses to separately image the coherence contributions. The technique can selectively follow the relevant electrons involved in the ultrafast dynamics and identify the confined molecular regions covered by their motion. It enables readily feasible measurements and can be straightforwardly extended to full three-dimensional imaging via X-ray and electron diffraction.
Effects of sulfurization time and H{sub 2}S concentration on electrical properties of Cu{sub 2}ZnSnS{sub 4} films prepared by sol–gel method
Highlights: • Cu{sub 2}ZnSnS{sub 4} (CZTS) films were prepared by sol–gel method following sulfurization. • The sulfurization time and H{sub 2}S concentration have the effects on the electrical properties. • The tin loss is increased with the increasing of the sulfurization time. • The secondary phases like ZnS make the electrical properties worse. • The CZTS films sulfurized at 5% H{sub 2}S for 90 min had the best electrical properties. - Abstract: Cu{sub 2}ZnSnS{sub 4} (CZTS) thin films have been successfully deposited by a sol–gel method and sulfurization process. The properties of the films were investigated by varying sulfurization time and H{sub 2}S concentration. X-ray diffraction and Raman spectra analyses revealed the formation of CZTS films with a tetragonal type kesterite structure. With increasing the sulfurization time and H{sub 2}S concentration, the intensity of the kesterite (1 1 2) peak became sharper. The stoichiometric ratios of the CZTS films were different from the precursors, which was due to Sn loss during the sulfurization process. The electrical resistivity and mobility of the films increased while the carrier concentration decreased with increasing the sulfurization time. The CZTS thin films sulfurized at 5% H{sub 2}S concentration for 90 min had the best opto-electrical properties with E{sub g} of 1.41 eV, resistivity of 3.64 Ω cm, carrier concentration of 1.11 × 10{sup 18} cm{sup −3} and mobility of 1.54 cm{sup 2}/(V s) at room temperature for PV application.
Direct Observations of a Dynamically Driven Phase Transition with in situ X-Ray Diffraction in a Simple Ionic Crystal.
Abstract not provided.
Crystal Growth and Characterization of the Narrow-Band-Gap Semiconductors OsPn 2 (Pn = P, As, Sb)
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