Chad M. Parish

Correlated optical measurements and plasmon mapping of silver nanorods.

Plasmonics is a rapidly growing field, yet imaging of the plasmonic modes in complex nanoscale architectures is extremely challenging. Here we obtain spatial maps of the localized surface plasmon modes of high-aspect-ratio silver nanorods using electron energy loss spectroscopy (EELS) and correlate to optical data and classical electrodynamics calculations from the exact same particles. EELS mapping is thus demonstrated to be an invaluable technique for elucidating complex and overlapping plasmon modes.

Role of alloying elements in nanostructured ferritic steels

Abstract The roles of the alloying elements in three nanostructured ferritic alloys (14YWT, MA957 and Eurofer 97) have been established through the characterisation of the microstructure by atom probe tomography and spectrum imaging in a transmission electron microscope. Cr, W, Mo, Ti and Y were found in the ferrite matrix and contributed to solid solution hardening. Ti, Y, C, O and N were found in high number densities of precipitates and nanoclusters both in the grain interior and on grain boundaries and thereby contributed to precipitation hardening. Cr, W and Mo were enriched at the intraparticle regions of the grain boundaries. The solute segregation and precipitation pinned the grain boundaries and contributed to the excellent creep properties of the alloys.

Novel cell design for combined in situ acoustic emission and x-ray diffraction study during electrochemical cycling of batteries

An in situ acoustic emission (AE) and x-ray diffraction cell for use in the study of battery electrode materials has been designed and tested. This cell uses commercially available coin cell hardware retrofitted with a metalized polyethylene terephthalate (PET) disk, which acts as both an x-ray window and a current collector. In this manner, the use of beryllium and its associated cost and hazards is avoided. An AE sensor may be affixed to the cell face opposite the PET window in order to monitor degradation effects, such as particle fracture, during cell cycling. Silicon particles, which were previously studied by the AE technique, were tested in this cell as a model material. The performance of these cells compared well with unmodified coin cells, while providing information about structural changes in the active material as the cell is repeatedly charged and discharged.

Advanced oxide dispersion strengthened and nanostructured ferritic alloys

Abstract Nanostructured ferritic alloy is a subcategory of oxide dispersion strengthened steels intended for advanced reactor applications. The complex ultrafine grained microstructure of an advanced nanostructured ferritic alloy, as determined by electron microscopy and atom probe tomography, is summarised. Three distinct populations of precipitates were observed: 20–50 nm Ti(N,O,C), 5–10 nm diameter Y2Ti2O7/Y2TiO5 and 1–4 nm diameter Ti,Y,O enriched nanoclusters. The first two populations were predominantly located along grain boundaries together with Cr, W and C segregation. A dense population of nanoclusters was observed both in the grain interior as well as on the grain boundaries. These nanoclusters are highly tolerant to high dose irradiation at elevated temperatures.

Nanocone Tip–Film Solar Cells with Efficient Charge Transport

Nanojunctions promise to provide higher charge transport efficiencies and less costly solar cell fabrication methods. We report a three-dimensional (3D) solar cell structure based on interdigitated nanojunctions formed with the tips of n-type ZnO nanocones embedded in a p-type polycrystalline (PX) CdTe film. This 3D nanocone tip-film cell, without optimization, enabled 3.2% power conversion efficiency, higher than that produced by a planar solar cell fabricated using the same materials. Reducing CdTe grain size and enriching the grain boundaries with chlorine improved the conversion efficiency for the tip-film structure. This higher conversion efficiency is attributable to improved charge transport in the nanojunction due to a combination of the high electric field generated in the CdTe and the utilization of the small junction area. The high field facilitates the extraction of minority carriers from the photoactive layer to the small junction region, while the use of the small junction area reduces the total electron recombination loss. The improved carrier transport in the nanocone tip-film junction implies that nanocone-based photovoltaic solar cells are capable of tolerating the imperfect materials produced using low-cost fabrication methods.

Multivariate statistics applications in phase analysis of STEM-EDS spectrum images

Spectrum imaging (SI) methods are displacing traditional spot analyses as the predominant paradigm for spectroscopic analysis with electron beam instrumentation. The multivariate nature of SI provides clear advantages for qualitative analysis of multiphase specimens relative to traditional gray-scale images acquired with non-spectroscopic signals, where different phases with similar average atomic number may exhibit the same intensity. However, with the improvement in qualitative analysis with the SI paradigm has come a decline in the quantitative analysis of the phases thus identified, since the spectra from individual pixels typically have insufficient counting statistics for proper quantification. The present paper outlines a methodology for quantitative analysis within the spectral imaging paradigm, which is illustrated through X-ray energy-dispersive spectroscopy (EDS) of a multiphase (Pb,La)(Zr,Ti)O(3) ceramic in scanning transmission electron microscopy (STEM). Statistical analysis of STEM-EDS SI is shown to identify the number of distinct phases in the analyzed specimen and to provide better segmentation than the STEM high-angle annular dark-field (HAADF) signal. Representative spectra for the identified phases are extracted from the segmented images with and without exclusion of pixels that exhibit spectral contributions from multiple phases, and subsequently quantified using Cliff-Lorimer sensitivity factors. The phase compositions extracted with the method while excluding pixels from multiple phases are found to be in good agreement with those extracted from user-selected regions of interest, while providing improved confidence intervals. Without exclusion of multiphase pixels, the extracted composition is found to be in poor statistical agreement with the other results because of systematic errors arising from the cross-phase spectral contamination. The proposed method allows quantification to be performed in the presence of discontinuous phase distributions and overlapping phases, challenges that are typical of many nanoscale analyses performed by STEM-EDS.

Scanning Cathodoluminescence Microscopy

Publisher Summary Cathodoluminescence (CL) is light emitted by a solid material because of irradiation by an electron beam. When the spectral distribution of light is studied, CL spectroscopy is performed. This chapter focuses on advances in CL instrumentation, theory, and application. CL is a valuable technique for studying the optical emission properties of semiconductor and insulating materials at a very fine spatial resolution. CL is an indispensable tool for the study of light emission from materials and the factors that improve or degrade it in the semiconductor and optoelectronic industries. CL is also heavily used in studies of mineralogy and geology. The basic physics that gives rise to the CL signal and the way the nature of the solid material under investigation changes the CL response is also presented in the chapter.

On the use of Monte Carlo modeling in the mathematical analysis of scanning electron microscopy–electron beam induced current data

Electron beam induced current (EBIC) is often used to evaluate minority carrier properties in semiconductors. Various mathematical models have been proposed; the most advanced is that of Bonard and Ganiere [J. Appl. Phys. 79, 6987 (1996)]. However, in order to apply this model to EBIC experiments, the lateral and depth distributions of the electron-hole-pair generation in the sample must be known. This letter presents a straightforward method based on Monte Carlo simulation of the electron beam interaction with the sample to evaluate these distribution parameters. A quantitative experimental example from a GaN-based light emitting diode is presented to test the proposed method.

Analysis of V defects in GaN-based light emitting diodes by scanning transmission electron microscopy and electron beam induced current

In the fabrication of InGaN∕GaN multiple quantum well light emitting diodes so-called V defects are common, but little is known about their electrical activity. Scanning transmission electron microscopy is capable of directly observing these defects, while electron beam induced current (EBIC) techniques can be used to probe electronic behavior of semiconductor defects. These techniques were combined to obtain localized measurements and our results indicate that V defects suppress the EBIC signal near the core of the defect and produce a displacement in the p-n junction location. Furthermore, the EBIC profile suggests that minority carrier diffusion lengths are longer inside the defect.

Flux threshold measurements of He-ion beam induced nanofuzz formation on hot tungsten surfaces

We report measurements of the energy dependence of flux thresholds and incubation fluences for He-ion induced nano-fuzz formation on hot tungsten surfaces at UHV conditions over a wide energy range using real-time sample imaging of tungsten target emissivity change to monitor the spatial extent of nano-fuzz growth, corroborated by ex situ SEM and FIB/SEM analysis, in conjunction with accurate ion-flux profile measurements. The measurements were carried out at the multicharged ion research facility (MIRF) at energies from 218 eV to 8.5 keV, using a high-flux deceleration module and beam flux monitor for optimizing the decel optics on the low energy MIRF beamline. The measurements suggest that nano-fuzz formation proceeds only if a critical rate of change of trapped He density in the W target is exceeded. To understand the energy dependence of the observed flux thresholds, the energy dependence of three contributing factors: ion reflection, ion range and target damage creation, were determined using the SRIM simulation code. The observed energy dependence can be well reproduced by the combined energy dependences of these three factors. The incubation fluences deduced from first visual appearance of surface emissivity change were (2–4) × 1023 m−2 at 218 eV, and roughly a factor of 10 less at the higher energies, which were all at or above the displacement energy threshold. The role of trapping at C impurity sites is discussed.