Characterization of Anomalous Grains in FeCo Magnetic Alloys.

Heat-treated FeCo-based magnetic alloys were characterized using a suite of electron microscopy techniques to gain insight into their structural properties. Electron channeling contrast imaging (ECCI) in the scanning electron microscope (SEM) found unique grains towards the outer edge of a FeCo sample with nonuniform background contrast. High-magnification ECCI imaging of these nonuniform grains revealed a weblike network of defects that were not observed in standard uniform background contrast grains. High-resolution electron backscattered diffraction (HR-EBSD) confirmed these defect structures to be dislocation networks and additionally found subgrain boundaries within the nonuniform contrast grains. The defect content within these grains suggests that they are unrecrystallized grains, and ECCI can be used as a rapid method to quantify unrecrystallized grains. To demonstrate the insight that can be garnered via ECCI on these unique grains, the sample was imaged before and after micro indentation. This experiment showed that slip bands propagate throughout the material until interacting with the dislocation networks, suggesting that these specific defects provide a barrier to plastic deformation. Taken together, these results show how ECCI can be used to better understand failure mechanisms in alloys and provides further evidence that dislocation networks play a critical role in the brittle failure of FeCo alloys.

Identification of Star Defects in Gallium Nitride with HREBSD and ECCI.

This paper characterizes novel "star" defects in GaN films grown with metal­organic vapor phase deposition (MOVPE) on GaN substrates with electron channeling contrast imaging (ECCI) and high-resolution electron backscatter diffraction (HREBSD). These defects are hundreds of microns in size and tend to aggregate threading dislocations at their centers. They are the intersection of six nearly ideal low-angle tilt boundaries composed of $\langle a\rangle$-type pyramidal edge dislocations, each on a unique slip system.

Nano-Cathodoluminescence Measurement of Asymmetric Carrier Trapping and Radiative Recombination in GaN and InGaN Quantum Disks.

The ability to characterize recombination and carrier trapping processes in group-III nitride-based nanowires is vital to further improvements in their overall efficiencies. While advances in scanning transmission electron microscope (STEM)-based cathodoluminescence (CL) have offered some insight into nanowire behavior, inconsistencies in nanowire emission along with CL detector limitations have resulted in the incomplete understanding in nanowire emission processes. Here, two nanowire heterostructures were explored with STEM-CL: a polarization-graded AlGaN nanowire light-emitting diode (LED) with a GaN quantum disk and a polarization-graded AlGaN nanowire with three different InGaN quantum disks. Most nanowires explored in this study did not emit. For the wires that did emit in both structures, they exhibited asymmetrical emission consistent with the polarization-induced electric fields in the barrier regions of the nano-LEDs. In the AlGaN/InGaN sample, two of the quantum disks exhibited no emission potentially due to the three-dimensional landscape of the sample or due to limitations in the CL detection.

Electrochemical Liquid Phase Epitaxy (ec-LPE): A New Methodology for the Synthesis of Crystalline Group IV Semiconductor Epifilms.

Deposition of epitaxial germanium (Ge) thin films on silicon (Si) wafers has been achieved over large areas with aqueous feedstock solutions using electrochemical liquid phase epitaxy (ec-LPE) at low temperatures (T ≤ 90 °C). The ec-LPE method uniquely blends the simplicity and control of traditional electrodeposition with the material quality of melt growth. A new electrochemical cell design based on the compression of a liquid metal electrode into a thin cavity that enables ec-LPE is described. The epitaxial nature, low strain character, and crystallographic defect content of the resultant solid Ge films were analyzed by electron backscatter diffraction, scanning transmission electron microscopy, high resolution X-ray diffraction, and electron channeling contrast imaging. The results here show the first step toward a manufacturing infrastructure for traditional crystalline inorganic semiconductor epifilms that does not require high temperature, gaseous precursors, or complex apparatus.

Manipulating acoustic and plasmonic modes in gold nanostars.

In this contribution experimental evidence of plasmonic edge modes and acoustic breathing modes in gold nanostars (AuNSs) is reported. AuNSs are synthesized by a surfactant-free, one-step wet-chemistry method. Optical extinction measurements of AuNSs confirm the presence of localized surface plasmon resonances (LSPRs), while electron energy-loss spectroscopy (EELS) using a scanning transmission electron microscope (STEM) shows the spatial distribution of LSPRs and reveals the presence of acoustic breathing modes. Plasmonic hot-spots generated at the pinnacle of the sharp spikes, due to the optically active dipolar edge mode, allow significant intensity enhancement of local fields and hot-electron injection, and are thus useful for size detection of small protein molecules. The breathing modes observed away from the apices of the nanostars are identified as stimulated dark modes - they have an acoustic nature - and likely originate from the confinement of the surface plasmon by the geometrical boundaries of a nanostructure. The presence of both types of modes is verified by numerical simulations. Both these modes offer the possibility of designing nanoplasmonic antennas based on AuNSs, which can provide information on both mass and polarizability of biomolecules using a two-step molecular detection process.

Heterodimeric Plasmonic Nanogaps for Biosensing.

We report the study of heterodimeric plasmonic nanogaps created between gold nanostar (AuNS) tips and gold nanospheres. The selective binding is realized by properly functionalizing the two nanostructures; in particular, the hot electrons injected at the nanostar tips trigger a regio-specific chemical link with the functionalized nanospheres. AuNSs were synthesized in a simple, one-step, surfactant-free, high-yield wet-chemistry method. The high aspect ratio of the sharp nanostar tip collects and concentrates intense electromagnetic fields in ultrasmall surfaces with small curvature radius. The extremities of these surface tips become plasmonic hot spots, allowing significant intensity enhancement of local fields and hot-electron injection. Electron energy-loss spectroscopy (EELS) was performed to spatially map local plasmonic modes of the nanostar. The presence of different kinds of modes at different position of these nanostars makes them one of the most efficient, unique, and smart plasmonic antennas. These modes are harnessed to mediate the formation of heterodimers (nanostar-nanosphere) through hot-electron-induced chemical modification of the tip. For an AuNS-nanosphere heterodimeric gap, the intensity enhancement factor in the hot-spot region was determined to be 106, which is an order of magnitude greater than the single nanostar tip. The intense local electric field within the nanogap results in ultra-high sensitivity for the presence of bioanalytes captured in that region. In case of a single BSA molecule (66.5 KDa), the sensitivity was evaluated to be about 1940 nm/RIU for a single AuNS, but was 5800 nm/RIU for the AuNS-nanosphere heterodimer. This indicates that this heterodimeric nanostructure can be used as an ultrasensitive plasmonic biosensor to detect single protein molecules or nucleic acid fragments of lower molecular weight with high specificity.

Electron Channeling Contrast Imaging for Rapid III-V Heteroepitaxial Characterization.

Misfit dislocations in heteroepitaxial layers of GaP grown on Si(001) substrates are characterized through use of electron channeling contrast imaging (ECCI) in a scanning electron microscope (SEM). ECCI allows for imaging of defects and crystallographic features under specific diffraction conditions, similar to that possible via plan-view transmission electron microscopy (PV-TEM). A particular advantage of the ECCI technique is that it requires little to no sample preparation, and indeed can use large area, as-produced samples, making it a considerably higher throughput characterization method than TEM. Similar to TEM, different diffraction conditions can be obtained with ECCI by tilting and rotating the sample in the SEM. This capability enables the selective imaging of specific defects, such as misfit dislocations at the GaP/Si interface, with high contrast levels, which are determined by the standard invisibility criteria. An example application of this technique is described wherein ECCI imaging is used to determine the critical thickness for dislocation nucleation for GaP-on-Si by imaging a range of samples with various GaP epilayer thicknesses. Examples of ECCI micrographs of additional defect types, including threading dislocations and a stacking fault, are provided as demonstration of its broad, TEM-like applicability. Ultimately, the combination of TEM-like capabilities - high spatial resolution and richness of microstructural data - with the convenience and speed of SEM, position ECCI as a powerful tool for the rapid characterization of crystalline materials.