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At least 1,261 records · Page 70

An in-situ study of magnetic domain structures in undercooled Fe-29.5 at. %Pd magnetostrictive alloys by Lorentz microscopy and electron holography

Understanding of correlation between magnetic domain structure and functional properties is of importance for the magnetic field driven phase transition (e.g., martensitic transformation) or microstructure variation (e.g., twin boundary motion) materials. In this work, we report a Fe-29.5 at. %Pd shape memory alloy treated by undercooling processing upon a degree of 320 K below the liquid temperature. The effect of high undercooling on the solidified microstructure and martensitic transformation temperatures was investigated. By in-situ Lorentz transmission electron microscopy and electron holography, magnetic domain structure and the field-induced domain wall motion behavior in as-cast and undercooled samples have been schematically studied. The irregular domain structure can be observed in these alloys. On the application of a field up to 300 Oe, the domain walls for both samples are able to move along the direction of the external magnetic field, but structural transition and rearrangement of variants are not observed in the undercooled alloy. The large magnetostriction of Fe-29.5 at. %Pd undercooled alloy originates from the irregular domain walls motion instead of the rearrangement of martensitic twin variants.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Note: A silicon-on-insulator microelectromechanical systems probe scanner for on-chip atomic force microscopy

A new microelectromechanical systems-based 2-degree-of-freedom (DoF) scanner with an integrated cantilever for on-chip atomic force microscopy (AFM) is presented. The silicon cantilever features a layer of piezoelectric material to facilitate its use for tapping mode AFM and enable simultaneous deflection sensing. Electrostatic actuators and electrothermal sensors are used to accurately position the cantilever within the x-y plane. Experimental testing shows that the cantilever is able to be scanned over a 10 μm × 10 μm window and that the cantilever achieves a peak-to-peak deflection greater than 400 nm when excited at its resonance frequency of approximately 62 kHz.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Transmission electron microscopy and ab initio calculations to relate interfacial intermixing and the magnetism of core/shell nanoparticles

Significant efforts towards understanding bi-magnetic core-shell nanoparticles are underway currently as they provide a pathway towards properties unavailable with single-phased systems. Recently, we have demonstrated that the magnetism of γ-Fe2O3/CoO core-shell nanoparticles, in particular, at high temperatures, originates essentially from an interfacial doped iron-oxide layer that is formed by the migration of Co{sup 2+} from the CoO shell into the surface layers of the γ-Fe2O3 core [Skoropata et al., Phys. Rev. B 89, 024410 (2014)]. To examine directly the nature of the intermixed layer, we have used high-resolution transmission electron microscopy (HRTEM) and first-principles calculations to examine the impact of the core-shell intermixing at the atomic level. By analyzing the HRTEM images and energy dispersive spectra, the level and nature of intermixing was confirmed, mainly as doping of Co into the octahedral site vacancies of γ-Fe2O3. The average Co doping depths for different processing temperatures (150 °C and 235 °C) were 0.56 nm and 0.78 nm (determined to within 5% through simulation), respectively, establishing that the amount of core-shell intermixing can be altered purposefully with an appropriate change in synthesis conditions. Through first-principles calculations, we find that the intermixing phase of γ-Fe2O3 with Co doping is ferromagnetic, with even higher magnetization as compared to that of pure γ-Fe2O3. In addition, we show that Co doping into different octahedral sites can cause different magnetizations. This was reflected in a change in overall nanoparticle magnetization, where we observed a 25% reduction in magnetization for the 235 °C versus the 150 °C sample, despite a thicker intermixed layer.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Application of microscopy technology in thermo-catalytic methane decomposition to hydrogen

Hydrogen production from the direct thermo-catalytic decomposition of methane is a promising alternative for clean fuel production because it produces pure hydrogen without any CO{sub x} emissions. However, thermal decomposition of methane can hardly be of any practical and empirical interest in the industry unless highly efficient and effective catalysts, in terms of both specific activity and operational lifetime have been developed. In this work, bimetallic Ni-Pd on gamma alumina support have been developed for methane cracking process by using co-precipitation and incipient wetness impregnation method. The calcined catalysts were characterized to determine their morphologies and physico-chemical properties by using Brunauer-Emmett-Teller method, Field Emission Scanning Electron Microscopy, Energy-dispersive X-ray spectroscopy and Thermogravimetric Analysis. The results suggested that that the catalyst which is prepared by the co-precipitation method exhibits homogeneous morphology, higher surface area, have uniform nickel and palladium dispersion and higher thermal stability as compared to the catalyst which is prepared by wet impregnation method. This characteristics are significant to avoid deactivation of the catalysts due to sintering and carbon deposition during methane cracking process.

36 MATERIALS SCIENCE↗

Visualization and quantification of magnetic nanoparticles into vesicular systems by combined atomic and magnetic force microscopy

We report a phenomenological approach for the quantification of the diameter of magnetic nanoparticles (MNPs) incorporated in non-ionic surfactant vesicles (niosomes) using magnetic force microscopy (MFM). After a simple specimen preparation, i.e., by putting a drop of solution containing MNPs-loaded niosomes on flat substrates, topography and MFM phase images are collected. To attempt the quantification of the diameter of entrapped MNPs, the method is calibrated on the sole MNPs deposited on the same substrates by analyzing the MFM signal as a function of the MNP diameter (at fixed tip-sample distance) and of the tip-sample distance (for selected MNPs). After calibration, the effective diameter of the MNPs entrapped in some niosomes is quantitatively deduced from MFM images.

36 MATERIALS SCIENCE↗

Comparative study of donor-induced quantum dots in Si nano-channels by single-electron transport characterization and Kelvin probe force microscopy

We comparatively study donor-induced quantum dots in Si nanoscale-channel transistors for a wide range of doping concentration by analysis of single-electron tunneling transport and surface potential measured by Kelvin probe force microscopy (KPFM). By correlating KPFM observations of donor-induced potential landscapes with simulations based on Thomas-Fermi approximation, it is demonstrated that single-electron tunneling transport at lowest gate voltages (for smallest coverage of screening electrons) is governed most frequently by only one dominant quantum dot, regardless of doping concentration. Doping concentration, however, primarily affects the internal structure of the quantum dot. At low concentrations, individual donors form most of the quantum dots, i.e., “donor-atom” quantum dots. In contrast, at high concentrations above metal-insulator transition, closely placed donors instead of individual donors form more complex quantum dots, i.e., “donor-cluster” quantum dots. The potential depth of these “donor-cluster” quantum dots is significantly reduced by increasing gate voltage (increasing coverage of screening electrons), leading to the occurrence of multiple competing quantum dots.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Experimental study of electric dipoles on an oxygen-adsorbed Si(100)-2 × 1 surface by non-contact scanning nonlinear dielectric microscopy

Oxygen-adsorption on a Si(100)-2 × 1 surface is investigated by using non-contact scanning nonlinear dielectric microscopy (NC-SNDM). On the Si(100)-2 × 1 surface exposed to oxygen (O{sub 2}) gas at room temperature, several variations in atomic configuration and electric dipole moment of dimers are observed. Models are proposed for oxygen adsorption which are consistent with the topographies and electric dipole moment distributions obtained by NC-SNDM.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Tailoring Si(100) substrate surfaces for GaP growth by Ga deposition: A low-energy electron microscopy study

For GaP-on-Si(100) heteroepitaxy, currently considered as a model system for monolithic integration of III–V semiconductors on Si(100), the surface steps of Si(100) have a major impact on the quality of the GaP film. Monoatomic steps cause antiphase domains in GaP with detrimental electronic properties. A viable route is to grow the III–V epilayer on single-domain Si(100) with biatomic steps, but preferably not at the expense of reduced terrace widths introduced by miscut substrates. We have performed in situ investigations of the influence of Ga deposition on the kinetics of surface steps and terraces of Si(100) at substrate temperatures above 600 °C by low-energy electron microscopy. Starting from nearly equally distributed T{sub A} and T{sub B} terraces of a two-domain Si(100) surface, submonolayer deposition of Ga results in a transformation into a surface dominated by T{sub A} terraces and biatomic D{sub A} steps. This transformation is reversible, and Si(100) with monoatomic steps is recovered upon termination of the Ga flux. Under conditions of higher coverages (but still below 0.25 monolayer), we observe restructuring into a surface with T{sub B} dominance, similar to the findings of Hara et al. [J. Appl. Phys. 98, 083515 (2005)]. The occurrence and mutual transformations of surface structures with different terrace and step structures in a narrow range of temperatures and Ga deposition rates is discussed.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Periodicity in bimodal atomic force microscopy

Periodicity is fundamental for quantification and the application of conservation principles of many important systems. Here, we discuss periodicity in the context of bimodal atomic force microscopy (AFM). The relationship between the excited frequencies is shown to affect and control both experimental observables and the main expressions quantified via these observables, i.e., virial and energy transfer expressions, which form the basis of the bimodal AFM theory. The presence of a fundamental frequency further simplifies the theory and leads to close form solutions. Predictions are verified via numerical integration of the equation of motion and experimentally on a mica surface.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Electrochemical strain microscopy time spectroscopy: Model and experiment on LiMn{sub 2}O{sub 4}

Electrochemical Strain Microscopy (ESM) can provide useful information on ionic diffusion in solids at the local scale. In this work, a finite element model of ESM measurements was developed and applied to commercial lithium manganese (III,IV) oxide (LiMn{sub 2}O{sub 4}) particles. ESM time spectroscopy was used, where a direct current (DC) voltage pulse locally disturbs the spatial distribution of mobile ions. After the pulse is off, the ions return to equilibrium at a rate which depends on the Li diffusivity in the material. At each stage, Li diffusivity is monitored by measuring the ESM response to a small alternative current (AC) voltage simultaneously applied to the tip. The model separates two different mechanisms, one linked to the response to DC bias and another one related to the AC excitation. It is argued that the second one is not diffusion-driven but is rather a contribution of the sum of several mechanisms with at least one depending on the lithium ion concentration explaining the relaxation process. With proper fitting of this decay, diffusion coefficients of lithium hosts could be extracted. Additionally, the effect of phase transition in LiMn{sub 2}O{sub 4} is taken into account, explaining some experimental observations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

In-situ piezoresponse force microscopy cantilever mode shape profiling

The frequency-dependent amplitude and phase in piezoresponse force microscopy (PFM) measurements are shown to be a consequence of the Euler-Bernoulli (EB) dynamics of atomic force microscope (AFM) cantilever beams used to make the measurements. Changes in the cantilever mode shape as a function of changes in the boundary conditions determine the sensitivity of cantilevers to forces between the tip and the sample. Conventional PFM and AFM measurements are made with the motion of the cantilever measured at one optical beam detector (OBD) spot location. A single OBD spot location provides a limited picture of the total cantilever motion, and in fact, experimentally observed cantilever amplitude and phase are shown to be strongly dependent on the OBD spot position for many measurements. In this work, the commonly observed frequency dependence of PFM response is explained through experimental measurements and analytic theoretical EB modeling of the PFM response as a function of both frequency and OBD spot location on a periodically poled lithium niobate sample. One notable conclusion is that a common choice of OBD spot location—at or near the tip of the cantilever—is particularly vulnerable to frequency dependent amplitude and phase variations stemming from dynamics of the cantilever sensor rather than from the piezoresponse of the sample.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Quantitative phase separation in multiferroic Bi{sub 0.88}Sm{sub 0.12}FeO{sub 3} ceramics via piezoresponse force microscopy

BiFeO{sub 3} (BFO) is a classical multiferroic material with both ferroelectric and magnetic ordering at room temperature. Doping of this material with rare-earth oxides was found to be an efficient way to enhance the otherwise low piezoelectric response of unmodified BFO ceramics. In this work, we studied two types of bulk Sm-modified BFO ceramics with compositions close to the morphotropic phase boundary (MPB) prepared by different solid-state processing methods. In both samples, coexistence of polar R3c and antipolar P{sub bam} phases was detected by conventional X-ray diffraction (XRD); the non-polar P{sub nma} or P{sub bnm} phase also has potential to be present due to the compositional proximity to the polar-to-non-polar phase boundary. Two approaches to separate the phases based on the piezoresponse force microscopy measurements have been proposed. The obtained fractions of the polar and non-polar/anti-polar phases were close to those determined by quantitative XRD analysis. The results thus reveal a useful method for quantitative determination of the phase composition in multi-phase ceramic systems, including the technologically most important MPB systems.

36 MATERIALS SCIENCE↗

Spatially resolved band alignments at Au-hexadecanethiol monolayer-GaAs(001) interfaces by ballistic electron emission microscopy

We study structural and electronic inhomogeneities in Metal—Organic Molecular monoLayer (OML)—semiconductor interfaces at the sub-nanometer scale by means of in situ Ballistic Electron Emission Microscopy (BEEM). BEEM imaging of Au/1-hexadecanethiols/GaAs(001) heterostructures reveals the evolution of pinholes density as a function of the thickness of the metallic top-contact. Using BEEM in spectroscopic mode in non-short-circuited areas, local electronic fingerprints (barrier height values and corresponding spectral weights) reveal a low-energy tunneling regime through the insulating organic monolayer. At higher energies, BEEM evidences new conduction channels, associated with hot-electron injection in the empty molecular orbitals of the OML. Corresponding band diagrams at buried interfaces can be thus locally described. The energy position of GaAs conduction band minimum in the heterostructure is observed to evolve as a function of the thickness of the deposited metal, and coherently with size-dependent electrostatic effects under the molecular patches. Such BEEM analysis provides a quantitative diagnosis on metallic top-contact formation on organic molecular monolayer and appears as a relevant characterization for its optimization.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Oxidation of GaSb(100) and its control studied by scanning tunneling microscopy and spectroscopy

Atomic-scale knowledge and control of oxidation of GaSb(100), which is a potential interface for energy-efficient transistors, are still incomplete, largely due to an amorphous structure of GaSb(100) oxides. We elucidate these issues with scanning-tunneling microscopy and spectroscopy. The unveiled oxidation-induced building blocks cause defect states above Fermi level around the conduction-band edge. By interconnecting the results to previous photoemission findings, we suggest that the oxidation starts with substituting second-layer Sb sites by oxygen. Adding small amount of indium on GaSb(100), resulting in a (4 × 2)-In reconstruction, before oxidation produces a previously unreported, crystalline oxidized layer of (1 × 3)-O free of gap states.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Choice of tip, signal stability, and practical aspects of piezoresponse-force-microscopy

Piezoresponse force-microscopy (PFM) has become the standard tool to investigate ferroelectrics on the micro- and nanoscale. However, reliability of PFM signals is often problematic and their quantification is challenging and thus not widely applied. Here, we present a study of the reproducibility of PFM signals and of the so-called PFM background signal which has been reported in the literature. We find that PFM signals are generally reproducible to certain extents. The PFM signal difference between 180° domains on periodically poled lithium niobate (PPLN) is taken as the reference signal in a large number of measurements, carried out in a low frequency regime (30-70 kHz). We show that in comparison to Pt coated tips, diamond coated tips exhibit improved signal stability, lower background signal, and less imaging artifacts related to PFM which is reflected in the spread of measurements. This is attributed to the improved mechanical stability of the conductive layer. The average deviation of the mean PFM signal is 38.3%, for a diamond coated tip. Although this deviation is relatively high, it is far better than values from the literature which showed a deviation of approx. 73.1%. Additionally, we find that the average deviation of the background signal from 0 is 11.6% of the PPLN domain contrast. Thus, the background signal needs to be taken into account when quantifying PFM signals and should be subtracted from PFM signals. Those results are important for quantification of PFM signals, since PPLN might be used for this purpose when PFM signals measured on PPLN are related to its macroscopic d{sub 33} coefficient. Finally, the crucial influence of sample polishing on PFM signals is shown and we recommend to use a multistep polishing route with a final step involving 200 nm sized colloidal silica particles.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Submicron mass spectrometry imaging of single cells by combined use of mega electron volt time-of-flight secondary ion mass spectrometry and scanning transmission ion microscopy

In order to better understand biochemical processes inside an individual cell, it is important to measure the molecular composition at the submicron level. One of the promising mass spectrometry imaging techniques that may be used to accomplish this is Time-of-Flight Secondary Ion Mass Spectrometry (TOF-SIMS), using MeV energy heavy ions for excitation. MeV ions have the ability to desorb large intact molecules with a yield that is several orders of magnitude higher than conventional SIMS using keV ions. In order to increase the spatial resolution of the MeV TOF-SIMS system, we propose an independent TOF trigger using a STIM (scanning transmission ion microscopy) detector that is placed just behind the thin transmission target. This arrangement is suitable for biological samples in which the STIM detector simultaneously measures the mass distribution in scanned samples. The capability of the MeV TOF-SIMS setup was demonstrated by imaging the chemical composition of CaCo-2 cells.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

InAlN high electron mobility transistor Ti/Al/Ni/Au Ohmic contact optimisation assisted by in-situ high temperature transmission electron microscopy

This paper correlates the micro-structural and electrical characteristics associated with annealing of metallic multi-layers typically used in the formation of Ohmic contacts to InAlN high electron mobility transistors. The multi-layers comprised Ti/Al/Ni/Au and were annealed via rapid thermal processing at temperatures up to 925 °C with electrical current-voltage analysis establishing the onset of Ohmic (linear IV) behaviour at 750–800 °C. In-situ temperature dependent transmission electron microscopy established that metallic diffusion and inter-mixing were initiated near a temperature of 500 °C. Around 800 °C, inter-diffusion of the metal and semiconductor (nitride) was observed, correlating with the onset of Ohmic electrical behaviour. The sheet resistance associated with the InAlN/AlN/GaN interface is highly sensitive to the anneal temperature, with the range depending on the Ti layer thickness. The relationship between contact resistivity and measurement temperature follow that predicted by thermionic field emission for contacts annealed below 850 °C, but deviated above this due to excessive metal-semiconductor inter-diffusion.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Superconducting scanning tunneling microscopy tips in a magnetic field: Geometry-controlled order of the phase transition

The properties of geometrically confined superconductors significantly differ from their bulk counterparts. Here, we demonstrate the geometrical impact for superconducting scanning tunneling microscopy (STM) tips, where the confinement ranges from the atomic to the mesoscopic scale. To this end, we compare the experimentally determined magnetic field dependence for several vanadium tips to microscopic calculations based on the Usadel equation. For our theoretical model of a superconducting cone, we find a direct correlation between the geometry and the order of the superconducting phase transition. Increasing the opening angle of the cone changes the phase transition from first to second order. Comparing our experimental findings to the theory reveals first and second order quantum phase transitions in the vanadium STM tips. In addition, the theory also explains experimentally observed broadening effects by the specific tip geometry.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗