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At least 1,711 records · Page 95

Antiferromagnetic order in CaK ( Fe 1 – x Ni x ) 4 As 4 and its interplay with superconductivity

The magnetic order in CaK(Fe 1–x Ni x ) 4 As 4 (1144) single crystals (x = 0.051 and 0.033) has been studied by neutron diffraction. We observe magnetic Bragg peaks associated with the same propagation vectors as found for the collinear stripe antiferromagnetic (AFM) order in the related BaFe 2 As 2 (122) compound. The AFM state in 1144 preserves tetragonal symmetry and only a commensurate, noncollinear structure with a hedgehog spin-vortex crystal (SVC) arrangement in the Fe plane and simple AFM stacking along the c direction is consistent with our observations. The SVC order is promoted by the reduced symmetry in the FeAs layer in the 1144 structure. The long-range SVC order coexists with superconductivity, however, similar to the doped 122 compounds, the ordered magnetic moment is gradually suppressed with the developing superconducting order parameter. Lastly, this supports the notion that both collinear and noncollinear magnetism and superconductivity are competing for the same electrons coupled by Fermi surface nesting in iron arsenide superconductors.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Rotation of X-ray polarization in the glitches of a silicon crystal monochromator

EXAFS studies on dilute samples are usually carried out by collecting the fluorescence yield using a large-area multi-element detector. This method is susceptible to the `glitches' produced by all single-crystal monochromators. Glitches are sharp dips or spikes in the diffracted intensity at specific crystal orientations. If incorrectly compensated, they degrade the spectroscopic data. Normalization of the fluorescence signal by the incident flux alone is sometimes insufficient to compensate for the glitches. Measurements performed at the state-of-the-art wiggler beamline I20-scanning at Diamond Light Source have shown that the glitches alter the spatial distribution of the sample's quasi-elastic X-ray scattering. Because glitches result from additional Bragg reflections, multiple-beam dynamical diffraction theory is necessary to understand their effects. Here, the glitches of the Si(111) four-bounce monochromator of I20-scanning just above the Ni K edge are associated with their Bragg reflections. A fitting procedure that treats coherent and Compton scattering is developed and applied to a sample of an extremely dilute (100 micromolal) aqueous solution of Ni(NO 3 ) 2 . The depolarization of the wiggler X-ray beam out of the electron orbit is modeled. The fits achieve good agreement with the sample's quasi-elastic scattering with just a few parameters. The X-ray polarization is rotated up to ±4.3° within the glitches, as predicted by dynamical diffraction. These results will help users normalize EXAFS data at glitches.

Sutter, John P.↗

Pattern-matching indexing of Laue and monochromatic serial crystallography data for applications in materials science

Serial crystallography data can be challenging to index, as each frame is processed individually, rather than being processed as a whole like in conventional X-ray single-crystal crystallography. An algorithm has been developed to index still diffraction patterns arising from small-unit-cell samples. The algorithm is based on the matching of reciprocal-lattice vector pairs, as developed for Laue microdiffraction data indexing, combined with three-dimensional pattern matching using a nearest-neighbors approach. As a result, large-bandpass data (e.g. 5–24 keV energy range) and monochromatic data can be processed, the main requirement being prior knowledge of the unit cell. Furthermore, angles calculated in the vicinity of a few theoretical and experimental reciprocal-lattice vectors are compared, and only vectors with the highest number of common angles are selected as candidates to obtain the orientation matrix. Global matching on the entire pattern is then checked. Four indexing options are available, two for the ranking of the theoretical reciprocal-lattice vectors and two for reducing the number of possible candidates. Furthermore, the algorithm has been used to index several data sets collected under different experimental conditions on a series of model samples. Additionally, knowing the crystallographic structure of the sample and using this information to rank the theoretical reflections based on the structure factors helps the indexing of large-bandpass data for the largest-unit-cell samples. For small-bandpass data, shortening the candidate list to determine the orientation matrix should be based on matching pairs of reciprocal-lattice vectors instead of triplet matching.

36 MATERIALS SCIENCE↗

Serial snapshot crystallography for materials science with SwissFEL

New opportunities for studying (sub)microcrystalline materials with small unit cells, both organic and inorganic, will open up when the X-ray free electron laser (XFEL) presently being constructed in Switzerland (SwissFEL) comes online in 2017. Our synchrotron-based experiments mimicking the 4%-energy-bandpass mode of the SwissFEL beam show that it will be possible to record a diffraction pattern of up to 10 randomly oriented crystals in a single snapshot, to index the resulting reflections, and to extract their intensities reliably. The crystals are destroyed with each XFEL pulse, but by combining snapshots from several sets of crystals, a complete set of data can be assembled, and crystal structures of materials that are difficult to analyze otherwise will become accessible. Even with a single shot, at least a partial analysis of the crystal structure will be possible, and with 10–50 femtosecond pulses, this offers tantalizing possibilities for time-resolved studies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Processing and characteristics of transparent Gd 3 TaO 7 polycrystalline ceramics

Transparent polycrystalline Gd 3 TaO 7 ceramics were successfully developed. A sol-gel process was used to synthesize Gd 3 TaO 7 powder with a uniform composition and an estimated average particle size of 100 nm. Simultaneous thermal gravimetric analysis and differential thermal analysis (TGA/DTA) was used to identify the decomposition sequence as a function of temperature for the as-synthesized sol-gel powders. Crystallization was confirmed by X-ray diffraction (XRD) and a single phase was achieved by calcining at 1000°C. The calcined powders were hot-pressed at 1400°C to achieve >96% theoretical density with closed pore structure followed by a hot isostatic pressing at 1400°C at 207 MPa to achieve a fully dense structure. Microstructural characterization shows a uniform grain size distribution with an average grain size of about 7 μm. In-line transmission measurements revealed high transparency in the red and infrared. Thermal conductivity was measured to be >1.6 W/mK at room temperature, decreasing to ~1.3 W/mK by 500°C. Dielectric properties remain stable with relative permittivity values just above 200 and loss tangents <0.005 up to 350°C.

36 MATERIALS SCIENCE↗

Equation of state and hyperfine parameters of high-spin bridgmanite in the Earth’s lower mantle by synchrotron X-ray diffraction and Mössbauer spectroscopy

In this study, we performed synchrotron X-ray diffraction (XRD) and Mössbauer spectroscopy (SMS) measurements on two single-crystal bridgmanite samples [ Embedded Image and Embedded Image ] to investigate the combined effect of Fe and Al on the hyperfine parameters, lattice parameters, and equation of state (EoS) of bridgmanite up to 130 GPa. Our SMS results show that Fe2+ and Fe3+ in Bm6 and Al-Bm11 are predominantly located in the large pseudo-dodecahedral sites (A-site) at lower-mantle pressures. The observed drastic increase in the hyperfine quadrupole splitting (QS) between 13 and 32 GPa can be associated with an enhanced local distortion of the A-site Fe2+ in Bm6. In contrast to Bm6, the enhanced lattice distortion and the presence of extremely high QS values of Fe2+ are not observed in Al-Bm11 at high pressures. Our results here support the notion that the occurrence of the extremely high QS component of approximately 4 mm/s in bridgmanite is due to the lattice distortion in the high-spin (HS) A-site Fe2+, instead of the occurrence of the intermediate-spin state. Both A-site Fe2+ and Fe3+ in Bm6 and Al-Bm11 remain in the HS state at lower-mantle pressures. Together with XRD results, we present the first experimental evidence that the enhanced lattice distortion of A-site Fe2+ does not cause any detectable variation in the EoS parameters, but is associated with anomalous variations in the bond length, tilting angle, and shear strain in the octahedra of Bm6. Analysis of the obtained EoS parameters of bridgmanite at lower-mantle pressures indicates that the substitution of Fe in bridgmanite will cause an enhanced density and a reduced bulk sound velocity (VΦ), whereas the Al and Fe substitution has a reduced effect on density and a negligible effect on VΦ. These experimental results provide new insight into the correlation between lattice, hyperfine, and EoS parameters of bridgmanite in the Earth’s lower mantle.

58 GEOSCIENCES↗

Adsorption and condensation of Cu on W single-crystal surfaces

The adsorption and condensation of Cu up to several monolayers in thickness on tungsten 110 and 100 single-crystal surfaces are studied by combining low-energy electron diffraction, Auger electron spectroscopy, thermal desorption spectroscopy, work-function measurements, and quartz microbalance thickness measurements in one experimental system. The results show drastic differences in the evolution of the structure, work function, and desorption behavior between 110 and 100 surfaces. These differences are understandable in terms of the atomic roughness of the surfaces.

Bauer, E.↗

Effect of abrasive grit size on wear of manganese-zinc ferrite under three-body abrasion

Wear experiments were conducted using replication electron microscopy and reflection electron diffraction to study abrasion and deformed layers produced in single-crystal Mn-Zn ferrites under three-body abrasion. The abrasion mechanism of Mn-Zn ferrite changes drastically with the size of abrasive grits. With 15-micron (1000-mesh) SiC grits, abrasion of Mn-Zn ferrite is due principally to brittle fracture; while with 4- and 2-micron (4000- and 6000-mesh) SiC grits, abrasion is due to plastic deformation and fracture. Both microcracking and plastic flow produce polycrystalline states on the wear surfaces of single-crystal Mn-Zn ferrites. Coefficient of wear, total thickness of the deformed layers, and surface roughness of the wear surfaces increase markedly with an increase in abrasive grit size. The total thicknesses of the deformed layers are 3 microns for the ferrite abraded by 15-micron SiC, 0.9 microns for the ferrite abraded by 4-micron SiC, and 0.8 microns for the ferrite abraded by 1-micron SiC.

Miyoshi, Kazuhisa↗

Structure and physical properties of RT{sub 2}Cd{sub 20} (R=rare earth, T=Ni, Pd) compounds with the CeCr{sub 2}Al{sub 20}-type structure

Eleven new compounds, R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Sm, Gd, Tb) and R Pd{sub 2}Cd{sub 20} (R=Ce, Pr, Sm), were grown as single crystals in high temperature cadmium-rich solutions. They crystallize in the cubic CeCr{sub 2}Al{sub 20}-type structure (Fd3{sup ¯}m, Z=8) as characterized by measurements of powder X-ray diffraction. Electrical resistivity, magnetization, and specific heat measurements were performed on R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Sm, Gd, Tb) single crystals. Whereas YNi{sub 2}Cd{sub 20} and LaNi{sub 2}Cd{sub 20} exhibit unremarkable metallic behavior, when magnetic moments from localized 4f electron states (Gd{sup 3+}–Tb{sup 3+}) are embedded into this host, they exhibit ferromagnetic order with values of the Curie temperature T{sub C} for R Ni{sub 2}Cd{sub 20} (R=Gd, and Tb) which scale with the de Gennes factor. - Graphical abstract: Specific heat divided by temperature C/T vs. T for single crystals of R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Gd, and Tb). Left inset: Low temperature C/T vs. T{sup 2} for LaNi{sub 2}Cd{sub 20}. The solid line represents a linear fit of the data. Right inset: Low-temperature C/T data vs. T for R=Ce–Nd, Gd, and Tb; magnetic ordering temperatures are indicated by arrows. - Highlights: • R Ni{sub 2}Cd{sub 20} (R=Y, La–Nd, Sm, Gd, Tb) single crystals synthesized for the first time. • R Pd{sub 2}Cd{sub 20} (R=Ce, Pr, Sm) single crystals synthesized for the first time. • Single crystals are of good metallurgical quality (large RRR values). • NdNi{sub 2}Cd{sub 20} orders antiferromagnetically at T{sub N}=1.5 K. • R Ni{sub 2}Cd{sub 20} (R=Sm, Gd, Tb) order ferromagnetically.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High pressure Laue diffraction and its application to study microstructural changes during the α → β phase transition in Si

Here, an approach using polychromatic x-ray Laue diffraction is described for studying pressure induced microstructural changes of materials under pressure. The advantages of this approach with respect to application of monochromatic x-ray diffraction and other techniques are discussed. Experiments to demonstrate the applications of the method have been performed on the α → β phase transition in Si at high pressures using a diamond anvil cell. We present the characterization of microstructures across the α–β phase transition, such as morphology of both the parent and product phases, relative orientation of single-crystals, and deviatoric strains. Subtle inhomogeneous strain of the single-crystal sample caused by lattice rotations becomes detectable with the approach.

47 OTHER INSTRUMENTATION↗

MOCVD Growth and Characterization of ZnSnN 2

Since the first few reports of its synthesis in 2011 and 20121-3, interest in ZnSnN 2 for diverse applications, including photovoltaics1,3,4, visible light photocatalysis5, and optoelectronics, has been growing. Novel nitride-based LED device designs promise high gains in efficiency at emission wavelengths into the green, amber and even red.6-8 Their realization requires the precise insertion of an ultrathin layer of ZnGeN 2 or ZnSnN 2 into the active region of an InGaAs-GaAs LED structure. While thin films of ZnSnN 2 have been synthesized by RF sputtering1,9 and by MBE 2,10,11, and thin films of ZnGeN 2 , ZnSiN 2 and their alloys by MOCVD, the synthesis of ZnSnN 2 thin films by MOCVD has not yet been reported. It is a challenging goal, given the narrow temperature window between efficient activation of ammonia and the thermal decomposition of ZnSnN 2 at near-atmospheric pressures. We report here the results of studies of ZnSnN 2 films grown on r- and c-plane sapphire substrates, GaN templates on sapphire, and In 0.15 Ga 0.85 N templates on GaN-on-sapphire, at temperatures from 500 °C to 560 °C, using tetramethyltin (TMSn), diethylzinc (DEZn), germane and ammonia. Chamber pressures were varied between 200 and 500 torr. In addition, the ratios of the cation precursors and the total cation-to-anion precursor ratios were varied. Single crystal growth, as evidenced by 2θ-ω x-ray diffraction scans, was achieved on all of these substrates. Wurtzitic (0002) ZnSnN 2 diffraction were observed at 2θ ~ 32.90 for the samples grown on c-sapphire, GaN (0001) and InGaN (0001) templates, and wurtzitic (11-20) peak at 2θ ~ 54.80 for the films grown on r-sapphire. Higher pressures and higher temperatures promoted better crystallinity and more continuous films, as revealed by scanning electron microscopy (SEM) images and 2θ-ω x-ray diffraction peak widths and intensities. Crystal quality was observed to be highly dependent on growth temperature. For example, in one series a 10 °C change in growth temperature resulting in a factor of 15 increase in diffraction peak intensity. SEM images show that films grown on the GaN templates had better uniformity in nucleation than those grown on sapphire. The presence of satellite peaks around the Bragg peak in the XRD 2θ-ω scan for a film grown on a GaN template, and the absence of satellite peaks for the films grown simultaneously on c- and r-sapphire, also indicate superior quality for the film grown on GaN. HAADF-STEM images of films grown on these templates showed smooth interfaces at the film-substrate boundary and show growth rates as high as 167 nm/h, considerably higher than reported previously for MBE growth.9,10 Electron diffraction patterns show single crystallinity. Rocking curves show FWHM as low as 0.100. RMS surfaces roughnesses, measured by atomic force microscopy, are of the order of 3 nm for 1µm x 1µm areas. Current work is focusing on optimizing growth on InGaN templates. These templates are promising for their relatively lower lattice mismatch with ZnSnN 2 . Their use is a next step toward producing LED device structures.

Jayatunga, Benthara Hewage Dinushi↗

Phase equilibria in the quasiternary system Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} and optical properties of (Ga{sub 55}In{sub 45}){sub 2}S{sub 300}, (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} single crystals

The quasiternary system Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} was investigated by differential thermal, X-ray diffraction analyses. The phase diagram of the Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} system and nine polythermal sections, isothermal section at 820 K and the liquidus surface projection were constructed. The existence of the large solid solutions ranges of binary and ternary compounds was established. The range of the existence of the quaternary phase AgGa{sub x}In{sub 5−x}S{sub 8} (2.25≤x≤2.85) at 820 K was determined. The single crystals (Ga{sub 55}In{sub 45}){sub 2}S{sub 300} and (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} were grown by a directional crystallization method from solution-melt. Optical absorption spectra in the 500–1600 nm range were recorded. The luminescence of the (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} single crystal shows a maximum at 1530 nm for the excitation wavelengths of 532 and 980 nm at 80 and 300 K. - Graphical abstract: Isothermal section of the quasiternary system Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3} at 820 K and normalized photoluminescence spectra of the single crystal (Ga{sub 54.59}In{sub 44.66}Er{sub 0.75}){sub 2}S{sub 300} at 300 K. - Highlights: • Isothermal section at 820 K, liquidus surface projection were built for Ag{sub 2}S–Ga{sub 2}S{sub 3}–In{sub 2}S{sub 3}. • Optical properties of single crystals were studied.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Diffraction of three-colour radiation on an acoustic wave

We study acousto-optic Bragg diffraction of three-colour radiation having wavelengths of 488, 514 and 633 nm on a single acoustic wave propagating in a TeO{sub 2} crystal. A technique is developed that allows one to find diffraction regimes with a proportional change in the intensity of all radiations by varying the acoustic power. According to the technique, radiation with a maximum wavelength has to be in strict Bragg synchronism with the acoustic wave, while other radiations diffract during the synchronism detuning. The results obtained using this technique are experimentally confirmed. (diffraction of light)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

In situ analysis of the nucleation of O- and Zn-polar ZnO nanowires using synchrotron-based X-ray diffraction

The selection of the polarity of ZnO nanowires grown by chemical bath deposition offers a great advantage for their integration into a wide variety of engineering devices. However, the nucleation process of ZnO nanowires and its dependence on their polarity is still unknown despite its importance for optimizing their morphology and properties and thus to enhance the related device performances. To tackle this major issue, we combine an in situ analysis of the nucleation process of O- and Zn-polar ZnO nanowires on O- and Zn-polar ZnO single crystals, respectively, using synchrotron radiation-based grazing incidence X-ray diffraction with ex situ transmission and scanning electron microscopy. We show that the formation of ZnO nanowires obeys three successive phases from the induction, through nucleation to growth phases. Additionally, the characteristics of each phase, including the nucleation temperature, the shape and dimension of nuclei, as well as their radial and axial development are found to depend on the polarity of ZnO nanowires. A comprehensive description reporting the dominant physicochemical processes in each phase and their dependence on the polarity of ZnO nanowires is presented, revisiting their formation process step-by-step. These findings provide a deeper understanding of the phenomena at work during the growth of ZnO nanowires by chemical bath deposition and open the perspective to develop a more accurate control of their properties at each step of the formation process.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Determining heterogeneous slip activity on multiple slip systems from single crystal orientation pole figures

A new experimental method to determine heterogeneity of shear strains associated with crystallographic slip in the bulk of ductile, crystalline materials is outlined. The method quantifies the time resolved evolution of misorientation within plastically deforming crystals using single crystal orientation pole figures (SCPFs) measured in-situ with X-ray diffraction. A multiplicative decomposition of the crystal kinematics is used to interpret the distributions of lattice plane orientation observed on the SCPFs in terms of heterogeneous slip activity (shear strains) on multiple slip systems. Here, to show the method’s utility, the evolution of heterogeneous slip is quantified in a silicon single crystal plastically deformed at high temperature at multiple load steps, with slip activity in sub-volumes of the crystal analyzed simultaneously.

36 MATERIALS SCIENCE↗

Ultrafast visualization of incipient plasticity in dynamically compressed matter

Plasticity is ubiquitous and plays a critical role in material deformation and damage; it inherently involves the atomistic length scale and picosecond time scale. A fundamental understanding of the elastic-plastic deformation transition, in particular, incipient plasticity, has been a grand challenge in high-pressure and high-strain-rate environments, impeded largely by experimental limitations on spatial and temporal resolution. Here, we report femtosecond MeV electron diffraction measurements visualizing the three-dimensional (3D) response of single-crystal aluminum to the ultrafast laser-induced compression. We capture lattice transitioning from a purely elastic to a plastically relaxed state within 5 ps, after reaching an elastic limit of ~25 GPa. Our results allow the direct determination of dislocation nucleation and transport that constitute the underlying defect kinetics of incipient plasticity. Large-scale molecular dynamics simulations show good agreement with the experiment and provide an atomic-level description of the dislocation-mediated plasticity.

36 MATERIALS SCIENCE↗

Real-time characterization of dislocation slip and twinning of shock-compressed molybdenum single crystals

Characterizing the fundamental micromechanisms activated during plastic deformation is critical to explain the macroscopic shock response of materials and develop accurate material models. In this paper, we investigate the orientation dependence, and the mediated slip and twin systems on [100] and [111] bcc molybdenum single crystals shock compressed up to 18 GPa with real-time Laue x-ray diffraction measurements. We report that dislocation slip along the {110} < 111 > and {112} < 111 > systems is the governing deformation mechanism during compression with negligible anisotropy observed at the Hugoniot state. Here, we provide real-time evidence that molybdenum undergoes deformation twinning along {11¯2} < 111 > during shock release.

36 MATERIALS SCIENCE↗