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At least 1,117 records · Page 62

Integration of microplasma with transmission electron microscopy: Real-time observation of gold sputtering and island formation

An in situ platform for characterizing plasma-materials interactions at the nanoscale in the transmission electron microscope (TEM) has been demonstrated. Integrating a DC microplasma device, having plane-parallel electrodes with a 25 nm thick Au film on both the cathode and anode and operating in 760 Torr of Ar, within a TEM provides real-time observation of Au sputtering and island formation with a spatial resolution of , 100 nm. Analyses of TEM and atomic force microscopy images show the growth of Au islands to proceed by a Stranski-Krastanov process at a rate that varies linearly with the discharge power and is approximately a factor of 3 larger than the predictions of a DC plasma sputtering model. The experiments reported here extend in situ TEM diagnostics to plasma-solid and plasma-liquid interactions.

METAMATERIALS↗

Charge collection kinetics on ferroelectric polymer surface using charge gradient microscopy

Here, a charge gradient microscopy (CGM) probe was used to collect surface screening charges on poly(vinylidene fluoride-trifluoroethylene) [P(VDF-TrFE)] thin films. These charges are naturally formed on unscreened ferroelectric domains in ambient condition. The CGM data were used to map the local electric current originating from the collected surface charges on the poled ferroelectric domains in the P(VDF-TrFE) thin films. Both the direction and amount of the collected current were controlled by changing the polarity and area of the poled domains. The endurance of charge collection by rubbing the CGM tip on the polymer film was limited to 20 scan cycles, after which the current reduced to almost zero. This degradation was attributed to the increase of the chemical bonding strength between the external screening charges and the polarization charges. Once this degradation mechanism is mitigated, the CGM technique can be applied to efficient energy harvesting devices using polymer ferroelectrics.

36 MATERIALS SCIENCE↗

Synchrotron-based X-ray fluorescence microscopy enables multiscale spatial visualization of ions involved in fungal lignocellulose deconstruction

Ions play an important role in the growth and development of filamentous fungi, particularly in the fungal decay process of lignocellulose materials. The role of ions in wood degradation, and more broadly fungal metabolism, have implications for diverse research disciplines ranging from plant pathology and forest ecology, to wood protection. Despite the importance of ions in both enzymatic and non-enzymatic fungal decay mechanisms, the spatial distribution of ions in wood and fungal hyphae during decay is not known. Here we employ synchrotron based X-ray fluorescence microscopy (XFM) to map physiologically relevant ions, such as K, Ca, Mn, Fe, and Zn, in wood being decayed by the model brown rot fungus Serpula lacrymans . Two-dimensional XFM maps were obtained to study the ion spatial distributions from mm to submicron length scales in wood and hyphae. Three-dimensional ion volume reconstructions with submicron spatial resolution were also acquired of wood cell walls and fungal hyphae, and an estimation of oxalate concentration at the microscale was made. Results show that the fungus actively transports some ions, such as Fe, into the wood and controls the distribution of ions at both the bulk wood and cellular length scales. Within the fungal hyphae, ion volume reconstructions show inhomogeneous ion distributions at the micron length scale and this localization may be indicative of both physiological status and requirements or in some cases, potentially sites associated with the initiation of metal-catalyzed wood degradation. Finally, these measurements illustrate how synchrotron based XFM is uniquely qualified for probing the role of ions in the growth and metabolic processes of filamentous fungi.

59 BASIC BIOLOGICAL SCIENCES↗

Loss tangent imaging: Theory and simulations of repulsive-mode tapping atomic force microscopy

An expression for loss tangent measurement of a surface in amplitude modulation atomic force microscopy is derived using only the cantilever phase and the normalized cantilever amplitude. This provides a direct measurement of substrate compositional information that only requires tuning of the cantilever resonance to provide quantitative information. Furthermore, the loss tangent expression incorporates both the lost and stored energy into one term that represents a fundamental interpretation of the phase signal in amplitude modulation imaging. Numerical solutions of a cantilever tip interacting with a simple Voigt modeled surface agree with the derived loss tangent to within a few percent.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Measurement of probe displacement to the thermal resolution limit in photonic force microscopy using a miniature quadrant photodetector

A photonic force microscope comprises of an optically trapped micro-probe and a position detection system to track the motion of the probe. Signal collection for motion detection is often carried out using the backscattered light off the probe-however, this mode has problems of low S/N due to the small backscattering cross sections of the micro-probes typically used. The position sensors often used in these cases are quadrant photodetectors. To ensure maximum sensitivity of such detectors, it would help if the detector size matched with the detection beam radius after the condenser lens (which for backscattered detection would be the trapping objective itself). To suit this condition, we have used a miniature displacement sensor whose dimensions makes it ideal to work with 1:1 images of micrometer-sized trapped probes in the backscattering detection mode. The detector is based on the quadrant photo-integrated chip in the optical pick-up head of a compact disc player. Using this detector, we measured absolute displacements of an optically trapped 1.1 {mu}m probe with a resolution of {approx}10 nm for a bandwidth of 10 Hz at 95% significance without any sample or laser stabilization. We characterized our optical trap for different sized probes by measuring the power spectrum for each probe to 1% accuracy, and found that for 1.1 {mu}m diameter probes, the noise in our position measurement matched the thermal resolution limit for averaging times up to 10 ms. We also achieved a linear response range of around 385 nm with cross talk between axes {approx_equal}4% for 1.1 {mu}m diameter probes. The detector has extremely high bandwidth (few MHz) and low optical power threshold-other factors that can lead to its widespread use in photonic force microscopy.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Transmission electron microscopy of the amorphization of copper indium diselenide by in situ ion irradiation

Copper indium diselenide (CIS), along with its derivatives Cu(In,Ga)(Se,S){sub 2}, is a prime candidate for use in the absorber layers of photovoltaic devices. Due to its ability to resist radiation damage, it is particularly well suited for use in extraterrestrial and other irradiating environments. However, the nature of its radiation hardness is not well understood. In this study, transmission electron microscopy (TEM) with in situ ion irradiation was used to monitor the dynamic microstructural effects of radiation damage on CIS. Samples were bombarded with 400 keV xenon ions to create large numbers of atomic displacements within the thickness of the TEM samples and thus explore the conditions under which, if any, CIS could be amorphized. By observing the impact of heavily damaging radiation in situ--rather than merely the end-state possible in ex situ experiments--at the magnifications allowed by TEM, it was possible to gain an understanding of the atomistic processes at work and the underlying mechanism that give rise to the radiation hardness of CIS. At 200 K and below, it was found that copper-poor samples could be amorphized and copper-rich samples could not. This difference in behavior is linked to the crystallographic phases that are present at different compositions. Amorphization was found to progress via a combination of one- and two-hit processes. The radiation hardness of CIS is discussed in terms of crystallographic structures/defects and the consequences these have for the ability of the material to recover from the effects of displacing radiation.

36 MATERIALS SCIENCE↗

Scanning tunneling microscopy reveals LiMnAs is a room temperature anti-ferromagnetic semiconductor

We performed scanning tunneling microscopy and spectroscopy on a LiMnAs(001) thin film epitaxially grown on an InAs(001) substrate by molecular beam epitaxy. While the in situ cleavage exposed only the InAs(110) non-polar planes, the cleavage continued into the LiMnAs thin layer across several facets. We combined both topography and current mappings to confirm that the facets correspond to LiMnAs. By spectroscopy we show that LiMnAs has a band gap. The band gap evidenced in this study, combined with the known Neel temperature well above room temperature, confirms that LiMnAs is a promising candidate for exploring the concepts of high temperature semiconductor spintronics based on antiferromagnets.

36 MATERIALS SCIENCE↗

Low temperature laser scanning microscopy of a superconducting radio-frequency cavity

An apparatus was created to obtain, for the first time, 2D maps of the surface resistance of the inner surface of an operating superconducting radio-frequency niobium cavity by a low-temperature laser scanning microscopy technique. This allows identifying non-uniformities of the surface resistance with a spatial resolution of about one order of magnitude better than with earlier methods. A signal-to-noise ratio of about 10 dB was obtained with 240 mW laser power and 1 Hz modulation frequency. The various components of the apparatus, the experimental procedure and results are discussed in details in this contribution.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

GaSb/GaAs quantum dot formation and demolition studied with cross-sectional scanning tunneling microscopy

We present a cross-sectional scanning tunneling microscopy study of GaSb/GaAs quantum dots grown by molecular beam epitaxy. Various nanostructures are observed as a function of the growth parameters. During growth, relaxation of the high local strain fields of the nanostructures plays an important role in their formation. Pyramidal dots with a high Sb content are often accompanied by threading dislocations above them. GaSb ring formation is favored by the use of a thin GaAs first cap layer and a high growth temperature of the second cap layer. At these capping conditions, strain-driven Sb diffusion combined with As/Sb exchange and Sb segregation remove the center of a nanostructure, creating a ring. Clusters of GaSb without a well defined morphology also appear regularly, often with a highly inhomogeneous structure which is sometimes divided up in fragments.

36 MATERIALS SCIENCE↗

Scanning secondary-electron microscopy on ferroelectric domains and domain walls in YMnO{sub 3}

Ferroelectric domain structures in YMnO{sub 3} single crystals on the hexagonal polar surface have been investigated by scanning electron microscopy in secondary electron emission mode. The experimental results demonstrate that the domain, as well as domain walls, can be clearly revealed under the operation voltages ranging from 0.6 to 3 kV. Evolution of domain contrasts arising from electron-beam irradiation can be mainly explained by the pyroelectric effect and related charging process. A rich variety of microstructure features of ferroelectric domains can be clearly revealed in YMnO{sub 3} by this high-resolution technique.

36 MATERIALS SCIENCE↗

A method to provide rapid in situ determination of tip radius in dynamic atomic force microscopy

We provide a method to characterize the tip radius of an atomic force microscopy in situ by monitoring the dynamics of the cantilever in ambient conditions. The key concept is that the value of free amplitude for which transitions from the attractive to repulsive force regimes are observed, strongly depends on the curvature of the tip. In practice, the smaller the value of free amplitude required to observe a transition, the sharper the tip. This general behavior is remarkably independent of the properties of the sample and cantilever characteristics and shows the strong dependence of the transitions on the tip radius. The main advantage of this method is rapid in situ characterization. Rapid in situ characterization enables one to continuously monitor the tip size during experiments. Further, we show how to reproducibly shape the tip from a given initial size to any chosen larger size. This approach combined with the in situ tip size monitoring enables quantitative comparison of materials measurements between samples. These methods are set to allow quantitative data acquisition and make direct data comparison readily available in the community.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Humidity-controlled preparation of frozen-hydrated biological samples for cryogenic coherent x-ray diffraction microscopy

Coherent x-ray diffraction microscopy (CXDM) has the potential to visualize the structures of micro- to sub-micrometer-sized biological particles, such as cells and organelles, at high resolution. Toward advancing structural studies on the functional states of such particles, here, we developed a system for the preparation of frozen-hydrated biological samples for cryogenic CXDM experiments. The system, which comprised a moist air generator, microscope, micro-injector mounted on a micromanipulator, custom-made sample preparation chamber, and flash-cooling device, allowed for the manipulation of sample particles in the relative humidity range of 20%-94%rh at 293 K to maintain their hydrated and functional states. Here, we report the details of the system and the operation procedure, including its application to the preparation of a frozen-hydrated chloroplast sample. Sample quality was evaluated through a cryogenic CXDM experiment conducted at BL29XUL of SPring-8. Taking the performance of the system and the quality of the sample, the system was suitable to prepare frozen-hydrated biological samples for cryogenic CXDM experiments.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Correlating whisker growth and grain structure on Sn-Cu samples by real-time scanning electron microscopy and backscattering diffraction characterization

Whiskers/hillocks grow out of Pb-free Sn coatings used in electronics manufacturing. To determine which grains form whiskers/hillocks, we use scanning electron microscopy and backscattering diffraction to simultaneously monitor the surface morphology and grain structure. To reduce surface roughness, we developed a ''peel-off'' method to prepare ultra-flat samples that were measured repeatedly while whiskers/hillocks formed. We find grains that form into whiskers/hillocks are present in the as-deposited film (i.e., not re-nucleated) and many have horizontal grain boundaries beneath them. Grain rotation during whisker/hillock formation means that measurements performed after the features grow do not indicate their initial grain orientations.

36 MATERIALS SCIENCE↗

Conductivity and structure of ErAs nanoparticles embedded in GaAs pn junctions analyzed via conductive atomic force microscopy

We have used conductive atomic force microscopy to investigate the influence of growth temperature on local current flow in GaAs pn junctions with embedded ErAs nanoparticles grown by molecular beam epitaxy. Three sets of samples, one with 1 ML ErAs deposited at different growth temperatures and two grown at 530 deg. C and 575 deg. C with varying ErAs depositions, were characterized. Statistical analysis of local current images suggests that the structures grown at 575 deg. C have about 3 times thicker ErAs nanoparticles than structures grown at 530 deg. C, resulting in degradation of conductivity due to reduced ErAs coverage. These findings explain previous studies of macroscopic tunnel junctions.

36 MATERIALS SCIENCE↗

In-situ transmission electron microscopy of partial-dislocation glide in 4H-SiC under electron radiation

Electron-radiation-enhanced glide of 30 Degree-Sign -Si(g) partial dislocations bringing about an expansion/shrinkage of Shockley-type stacking faults in 4H-SiC was observed in-situ by transmission electron microscopy. Geometrical kinks on 30 Degree-Sign -Si(g) partials did not migrate in the dark, indicating that the kink migration is enhanced by electron irradiation. The direction of the enhanced glide was reversible depending on the irradiation intensity, which can be interpreted in terms of a sign reversal of the driving force originating in the effective stacking fault energy variable with the irradiation intensity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Direct Determination of the Effect of Strain on Domain Morphology in Ferroelectric Superlattices with Scanning Probe Microscopy

A variant of piezo force microscopy was used to characterize the effect of strain on polarization in [(BaTiO3)n/(SrTiO3)m]p superlattices. The measurements were compared to theoretical predictions based on phase-field calculations. When polarization is constrained to be perpendicular to the substrate, the measured polarization and domain morphology agree quantitatively with the predictions. This case allows the presence of an internal electric field in the thin film to be identified. The measured trend in piezoelectric response with strain state was in qualitative agreement with predictions and the differences were consistent with the presence of internal electrical fields. Clear differences in domain morphology with strain were observed and in some cases the lateral anisotropic strain appeared to influence the domain morphology. The differences in magnitude and morphology were attributed to the internal electric fields and anisotropic strains.

effect of strain↗

Luminescence-based magnetic imaging with scanning x-ray transmission microscopy

We demonstrate the imaging of the magnetic domain configuration of cobalt structures fabricated on MgO(001) using x-ray induced optical luminescence in a scanning transmission microscope. The technique relies on the measurement of the magnetization-dependent x-ray absorption probed by the optical luminescence radiated from the MgO substrate and induced by the x-rays transmitted through the magnetic layer. This method enables the measurement of the electronic and magnetic spectroscopic properties of single crystalline layers and buried heterostructures with nanometer lateral resolution and elemental sensitivity and opens scanning transmission x-ray microscopy to materials which cannot be grown on membranes or as freestanding thin films.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗