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At least 73 records · Page 4

In situ transmission electron microscopy observation of ZnO polar and non-polar surfaces structure evolution under electron beam irradiation

In this paper, using in situ transmission electron microscopy, we investigated the dynamic reconstruction and evolution of ZnO polar and non-polar surfaces under high-energy electron beam irradiation. Electron beam radiolysis creates oxygen vacancies and a Zn rich (0001) surface. Positive polar charges at the (0001) surface expel loosely bonded Zn ions to diffuse away from the (0001) polar surface. As a result, mass loss was observed around the (0001) surface. Dehydration by the electron beam breaks the charge balance on the ( 000 1 ¯ ) polar surface. The negative charges on the ( 000 1 ¯ ) surface suppress the radiolysis effect and further absorb Zn ions to the surface to neutral the polar charges. The ideal stacking sequences of Zn ions in hexagonal ZnO structure can be considered as ABAB… along its c axis, while the absorbed individual Zn ion on the ( 000 1 ¯ ) surface occupies the C site to form three bonds with surface O ions beneath, instead of one bond in the ideal structure. With more Zn ion absorption and surface oxidization, new nanocrystals grow up from the ( 000 1 ¯ ) polar surface. Finally, new nanocrystals nucleated at the ( 01 1 ¯ 0 ) non-polar surface are driven by the electric field of the polar charges as well, for the Zn ions were always observed to absorb on the negatively charged [ 000 1 ¯ ] end of the newly formed ( 01 1 ¯ 0 ) surface layer.

74 ATOMIC AND MOLECULAR PHYSICS↗

Growth Dynamics and Electron Reflectivity in Ultrathin Films of Chiral Heptahelicene on Metal (100) Surfaces Studied by Spin-Polarized Low Energy Electron Microscopy

Interaction of electrons with chiral matter gives rise to interesting phenomena such as the chirality-induced spin selectivity. The interdependence of reflectivity of spin-polarized low energy electrons and the absolute handedness of chiral molecules is investigated. First, the growth of homochiral films of helical aromatic hydrocarbons, so-called helicenes, on a Cu(100) surface is studied by means of low energy electron microscopy and scanning tunneling microscopy in ultrahigh vacuum. As soon as the coverage exceeds one monolayer, double-layer nucleation and growth is favored such that depletion in the first layer occurs. Spatially resolved work function measurements show that second-layer patches have a lower work function than first-layer areas. Reflectivity spectra of spin-polarized electrons do not show any asymmetry between homochiral films of the enantiomers. Laterally resolved work function measurements do not confirm work function differences such as those reported earlier for photoelectron studies of chiral peptide films on ferromagnetic substrates.

36 MATERIALS SCIENCE↗

Crystallographic texture and microstructural changes in fusion welds of recrystallized Zry-4 rolled plates

This study presents a detailed characterization of the microstructural and crystallographic texture changes observed in the transition region in a weld between two Zircaloy-4 cold rolled and recrystallized plates. The microstructural study was performed by optical microscopy under polarized light and scanning electron microscopy (SEM). Texture changes were characterized at different lengthscales: in the micrometric size, orientation imaging maps (OIM) were constructed by electron backscatter diffraction (EBSD), in the millimetre scale, high energy XRD experiments were done at the Advanced Photon Source (USA) and compared to neutron diffraction texture determinations performed in the HIPPO instrument at Los Alamos National Laboratory. In the heat affected zone (HAZ) we observed the development of Widmanstätten microstructures, typical of the α( hcp ) to β( bcc ) phase transformation. Associated with these changes a rotation of the c-poles is found in the HAZ and fusion zone. While the base material shows the typical texture of a cold rolled plate, with their c-poles pointing 35° apart from the normal direction of the plate in the normal-transversal line, in the HAZ, c-poles align along the transversal direction of the plate and then re-orient along different directions, all of these changes occurring within a lengthscale in the order of mm. The evolution of texture in this narrow region was captured by both OIM and XRD, and is consistent with previous measurements done by Neutron Diffraction in the HIPPO diffractometer at Los Alamos National Laboratory, USA. The microstructural and texture changes along the HAZ were interpreted as arising due to the effect of differences in the cooling rate and β grain size on the progress of the different α variants during transformation. Fast cooling rates and large β grains are associated to weak variant selection during the β–>α transformation, while slow cooling rates and fine β grains result in strong variant selection.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Direct imaging of coexisting ordered and frustrated sublattices in artificial ferromagnetic quasicrystals

Here, we have used scanning electron microscopy with polarization analysis and photoemission electron microscopy to image the two-dimensional magnetization of permalloy films patterned into Penrose P2 tilings (P2T). The interplay of exchange interactions in asymmetrically coordinated vertices and short-range dipole interactions among connected film segments stabilize magnetically ordered, spatially distinct sublattices that coexist with frustrated sublattices at room temperature. Numerical simulations that include long-range dipole interactions between sublattices agree with images of as-grown P2T samples and predict a magnetically ordered ground state for a two-dimensional quasicrystal lattice of classical Ising spins.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Observation and implications of magnetic domains in lateral spin valves

Co/Cu/Co lateral spin valves (LSV), with Co being the topmost layer, are in situ prepared and measured under ultrahigh vacuum conditions. The clean process yields a non-local spin signal of 0.9 m{Omega}. Scanning electron microscopy with polarization analysis (SEMPA) reveals domain structures in both magnetic electrodes that depend on the LSV dimensions. The spin signal correlates to SEMPA images as well as the anisotropic magnetoresistance of both Co magnets, revealing a strong impact of multi-domain states on the spin signal.

36 MATERIALS SCIENCE↗

Engineered magnetic domain textures in exchange bias bilayer systems

A magnetic domain texture has been deterministically engineered in a topographically flat exchange-biased (EB) thin film system. The texture consists of long-range periodically arranged unit cells of four individual domains, characterized by individual anisotropies, individual geometry, and with non-collinear remanent magnetizations. The texture has been engineered by a sequence of light-ion bombardment induced magnetic patterning of the EB layer system. The magnetic texture's in-plane spatial magnetization distribution and the corresponding domain walls have been characterized by scanning electron microscopy with polarization analysis (SEMPA). The influence of magnetic stray fields emerging from neighboring domain walls and the influence of the different anisotropies of the adjacent domains on the Néel type domain wall core's magnetization rotation sense and widths were investigated. It is shown that the usual energy degeneracy of clockwise and counterclockwise rotating magnetization through the walls is revoked, suppressing Bloch lines along the domain wall. Estimates of the domain wall widths for different domain configurations based on material parameters determined by vibrating sample magnetometry were quantitatively compared to the SEMPA data.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Polarization-resolved second-harmonic generation microscopy as a method to visualize protein-crystal domains

Polarization-resolved second-harmonic generation microscopy is applied to the identification of multiple crystalline domains within protein-crystal samples. Polarization-resolved second-harmonic generation (PR-SHG) microscopy is described and applied to identify the presence of multiple crystallographic domains within protein-crystal conglomerates, which was confirmed by synchrotron X-ray diffraction. Principal component analysis (PCA) of PR-SHG images resulted in principal component 2 (PC2) images with areas of contrasting negative and positive values for conglomerated crystals and PC2 images exhibiting uniformly positive or uniformly negative values for single crystals. Qualitative assessment of PC2 images allowed the identification of domains of different internal ordering within protein-crystal samples as well as differentiation between multi-domain conglomerated crystals and single crystals. PR-SHG assessments of crystalline domains were in good agreement with spatially resolved synchrotron X-ray diffraction measurements. These results have implications for improving the productive throughput of protein structure determination through early identification of multi-domain crystals.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A microfluidic platform for pharmaceutical salt screening

We describe a microfluidic platform comprised of 48 wells to screen for pharmaceutical salts. Solutions of pharmaceutical parent compounds (PCs) and salt formers (SFs) are mixed on-chip in a combinatorial fashion in arrays of 87.5-nanolitre wells, which constitutes a drastic reduction of the volume of PC solution needed per condition screened compared to typical high throughput pharmaceutical screening approaches. Nucleation and growth of salt crystals is induced by diffusive and/or convective mixing of solutions containing, respectively, PCs and SFs in a variety of solvents. Here, to enable long term experiments, solvent loss was minimized by reducing the thickness of the absorptive polymeric material, polydimethylsiloxane (PDMS), and by using solvent impermeable top and bottom layers. Additionally, well isolation was enhanced via the incorporation of pneumatic valves that are closed at rest. Brightfield and polarized light microscopy and Raman spectroscopy were used for on-chip analysis and crystal identification. Using a gold-coated glass substrate and minimizing the thickness of the PDMS control layer drastically improved the signal-to-noise ratio for Raman spectra. Two drugs, naproxen (acid) and ephedrine (base), were used for validation of the platform's ability to screen for salts. Each PC was mixed combinatorially with potential SFs in a variety of solvents. Crystals were visualized using brightfield polarized light microscopy. Subsequent on-chip analyses of the crystals with Raman spectroscopy identified four different naproxen salts and five different ephedrine salts.

47 OTHER INSTRUMENTATION↗

Dynamic piezoresponse force microscopy: Spatially resolved probing of polarization dynamics in time and voltage domains

An approach for probing dynamic phenomena during hysteresis loop measurements in piezoresponse force microscopy (PFM) is developed. Dynamic PFM (D-PFM) necessitates development of 5-dimensional (5D) data acquisition protocols and associated methods for analysis and visualization of multidimensional data. Using a combination of multivariate statistical analysis and phenomenological fitting, we explore dynamic behavior during polarization switching in model ferroelectric films with dense ferroelastic domain structures and in ferroelectric capacitors. In polydomain films, multivariate analysis of the switching data suggests that ferroelectric and ferroelastic components can be decoupled and time dynamics can be explored. In capacitors, a strong correlation between polarization dynamics and microstructure is observed. The future potential of D-PFM for probing time-dependent hysteretic phenomena in ferroelectrics and ionic systems is discussed.

Dynamic piezoresponse force microscopy↗

Effect of capping material on interfacial ferromagnetism in FeRh thin films

The role of the capping material in stabilizing a thin ferromagnetic layer at the interface between a FeRh film and cap in the nominally antiferromagnetic phase at room temperature was studied by x-ray magnetic circular dichroism in photoemission electron microscopy and polarized neutron reflectivity. These techniques were used to determine the presence or absence of interfacial ferromagnetism (FM) in films capped with different oxides and metals. Chemically stable oxide caps do not generate any interfacial FM while the effect of metallic caps depends on the element, showing that interfacial FM is due to metallic interdiffusion and the formation of a ternary alloy with a modified antiferromagnetic to ferromagnetic transition temperature.

36 MATERIALS SCIENCE↗

Novel technique for spatially resolved imaging of molecular bond orientations using x-ray birefringence

Birefringence has been observed in anisotropic materials transmitting linearly polarized X-ray beams tuned close to an absorption edge of a specific element in the material. Synchrotron bending magnets provide X-ray beams of sufficiently high brightness and cross section for spatially resolved measurements of birefringence. The recently developed X-ray Birefringence Imaging (XBI) technique has been successfully applied for the first time using the versatile test beamline B16 at Diamond Light Source. Orientational distributions of the C–Br bonds of brominated “guest” molecules within crystalline “host” tunnel structures (in thiourea or urea inclusion compounds) have been studied using linearly polarized incident X-rays near the Br K-edge. Imaging of domain structures, changes in C–Br bond orientations associated with order-disorder phase transitions, and the effects of dynamic averaging of C–Br bond orientations have been demonstrated. The XBI setup uses a vertically deflecting high-resolution double-crystal monochromator upstream from the sample and a horizontally deflecting single-crystal polarization analyzer downstream, with a Bragg angle as close as possible to 45°. In this way, the ellipticity and rotation angle of the polarization of the beam transmitted through the sample is measured as in polarizing optical microscopy. The theoretical instrumental background calculated from the elliptical polarization of the bending-magnet X-rays, the imperfect polarization discrimination of the analyzer, and the correlation between vertical position and photon energy introduced by the monochromator agrees well with experimental observations. The background is calculated analytically because the region of X-ray phase space selected by this setup is sampled inefficiently by standard methods.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Kinetics of linear domains in LiNbO{sub 3} single crystals polarized by scanning probe microscopy

Growth and decay processes of linear domains in lithium niobate single crystals fabricated utilizing scanning probe microscopy were investigated. It is found that the initial configuration of linear domains is dependent on the fabrication parameters as scan velocity and voltage. The linear domains decay at the part where the domain width is small for two different processes. A comparison of critical stable domain size between dot and linear domains was carried out. The critical linear domain width is 0.7 times as large as the critical diameter of dot domain at the same sample thickness due to their smaller surface energy.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Thin film processing of photorefractive BaTiO3

During the period covered by this report, October 11, 1991 through October 10, 1992, the research has progressed in a number of different areas. The sol-gel technique was initially studied and experimentally evaluated for depositing films of BaTiO3. The difficulties with the precursors and the poor quality of the films deposited lead to the investigation of pulsed laser deposition as an alternative approach. The development of the pulsed laser deposition technique has resulted in continuous improvements to the quality of deposited films of BaTiO3. The initial depositions of BaTiO3 resulted in amorphous films, however, as the pulsed laser deposition technique continued to evolve, films were deposited in the polycrystalline state, then the textured polycrystalline state, and most recently heteroepitaxial films have also been successfully deposited on cubic (100) oriented SrTiO3 substrates. A technique for poling samples at room temperature and in air is also undergoing development with some very preliminary but positive results. The analytical techniques, which include x-ray diffraction, ferroelectric analysis, UV-Vis spectrophotometry, scanning electron microscopy with x-ray compositional analysis, optical and polarized light microscopy, and surface profilometry have been enhanced to allow for more detailed evaluation of the samples. In the area of optical characterization, a pulsed Nd:YAG laser has been incorporated into the experimental configuration. Now data can also be acquired within various temporal domains resulting in more detailed information on the optical response of the samples and on their photorefractive sensitivity. The recent establishment of collaborative efforts with two departments at Johns Hopkins University and the Army Research Lab at Fort Belvoir has also produced preliminary results using the metallo-organic decomposition technique as an alternative method for thin film processing of BaTiO3. RF and DC sputtering is another film deposition approach that should be initiated in the near future. Other techniques for optical characterization, which may even allow for intragrannular (within single grains) investigations, are also being considered.

Schuster, Paul R.↗

Crawler Solids Unknown Analysis

Crawler Transporter (CT) #2 has been undergoing refurbishment to carry the Space Launch System (SLS). After returning to normal operation, multiple filters of the gear box lubrication system failed/clogged and went on bypass during a test run to the launch pad. Analysis of the filters was done in large part with polarized light microscopy (PLM) to identify the filter contaminates and the source of origin.

Polarized Light Microscopy↗

Field-driven sense elements for chirality-dependent domain wall detection and storage

A method for locally sensing and storing data of transverse domain wall chirality in planar nanowire logic and memory systems is presented. Patterned elements, in close proximity to the nanowires, respond to the asymmetry in the stray field from the domain wall to produce a chirality-dependent response. When a bias field is applied, a stray field-assisted reversal of the element magnetization results in a reversed remanent state, measurable by scanning electron microscopy with polarization analysis (SEMPA). The elements are designed as triangles with tips pointing toward the nanowire, allowing the shape anisotropy to be dominated by the base but having a portion with lower volume and lower energy barrier closest to the domain wall. Micromagnetic modeling assists in the design of the nanowire-triangle systems and experiments using SEMPA confirm the importance of aspect ratio and spacing given a constant bias field magnitude.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Magnetic surface domain imaging of uncapped epitaxial FeRh(001) thin films across the temperature-induced metamagnetic transition

The surface magnetic domain structure of uncapped epitaxial FeRh/MgO(001) thin films was imaged by in-situ scanning electron microscopy with polarization analysis (SEMPA) at various temperatures between 122 and 450 K. This temperature range covers the temperature-driven antiferromagnetic-to-ferromagnetic phase transition in the body of the films that was observed in-situ by means of the more depth-sensitive magneto-optical Kerr effect. The SEMPA images confirm that the interfacial ferromagnetism coexisting with the antiferromagnetic phase inside the film is an intrinsic property of the FeRh(001) surface. Furthermore, the SEMPA data display a reduction of the in-plane magnetization occuring well above the phase transition temperature which, thus, is not related to the volume expansion at the phase transition. This observation is interpreted as a spin reorientation of the surface magnetization for which we propose a possible mechanism based on temperature-dependent tetragonal distortion due to different thermal expansion coefficients of MgO and FeRh.

36 MATERIALS SCIENCE↗