Sub-surface Imaging of Porous GaN Distributed Bragg Reflectors via Backscattered Electrons

In this article, porous GaN distributed Bragg reflectors (DBRs) were fabricated by epitaxy of undoped/doped multilayers followed by electrochemical etching. We present backscattered electron scanning electron microscopy (BSE-SEM) for sub-surface plan-view imaging, enabling efficient, non-destructive pore morphology characterization. In mesoporous GaN DBRs, BSE-SEM images the same branching pores and Voronoi-like domains as scanning transmission electron microscopy. In microporous GaN DBRs, micrographs were dominated by first porous layer features (45 nm to 108 nm sub-surface) with diffuse second layer (153 nm to 216 nm sub-surface) contributions. The optimum primary electron landing energy (LE) for image contrast and spatial resolution in a Zeiss GeminiSEM 300 was approximately 20 keV. BSE-SEM detects porosity ca. 295 nm sub-surface in an overgrown porous GaN DBR, yielding low contrast that is still first porous layer dominated. Imaging through a ca. 190 nm GaN cap improves contrast. We derived image contrast, spatial resolution, and information depth expectations from semi-empirical expressions. These theoretical studies echo our experiments as image contrast and spatial resolution can improve with higher LE, plateauing towards 30 keV. BSE-SEM is predicted to be dominated by the uppermost porous layer’s uppermost region, congruent with experimental analysis. Most pertinently, information depth increases with LE, as observed

Sub-surface imaging of porous GaN distributed Bragg reflectors via backscattered electrons

In this article, porous GaN distributed Bragg reflectors (DBRs) were fabricated by epitaxy of undoped/doped multilayers followed by electrochemical etching. We present backscattered electron scanning electron microscopy (BSE-SEM) for sub-surface plan-view imaging, enabling efficient, non-destructive pore morphology characterization. In mesoporous GaN DBRs, BSE-SEM images the same branching pores and Voronoi-like domains as scanning transmission electron microscopy. In microporous GaN DBRs, micrographs were dominated by first porous layer features (45 nm to 108 nm sub-surface) with diffuse second layer (153 nm to 216 nm sub-surface) contributions. The optimum primary electron landing energy (LE) for image contrast and spatial resolution in a Zeiss GeminiSEM 300 was approximately 20 keV. BSE-SEM detects porosity ca. 295 nm sub-surface in an overgrown porous GaN DBR, yielding low contrast that is still first porous layer dominated. Imaging through a ca. 190 nm GaN cap improves contrast. We derived image contrast, spatial resolution, and information depth expectations from semi-empirical expressions. These theoretical studies echo our experiments as image contrast and spatial resolution can improve with higher LE, plateauing towards 30 keV. BSE-SEM is predicted to be dominated by the uppermost porous layer's uppermost region, congruent with experimental analysis. Most pertinently, information depth increases with LE, as observed

Multi-scale characterization of ceramic inert-substrate-supported and co-sintered solid oxide fuel cells

Understanding cell performance is essential for selecting cell components and the processing parameters for solid oxide fuel cells. The scale of relevant microstructural features in electrodes, electrolyte and supporting substrate covers several orders of magnitude. This contribution will demonstrate how advanced correlative multi-scale tomography can be used to identify those parameters: ranging from millimeter to nanometer scale. We employ optical microscopy, X-ray computed tomography (μ-CT), focused ion beam-scanning electron microscopy tomography and energy-dispersive X-ray spectroscopy– scanning transmission electron microscopy. Additional investigations by selected area electron diffraction allow a determination of the underlying crystal structures. An SOFC design based on the co-sintering of an inert substrate with various functional layers on top is used as a blueprint, allowing further methodological development. The effect of interdiffusion between phases and development of secondary phases on microstructure and chemical composition will be shown. Furthermore, porosity and tortuosity extracted individually from all porous layers will allow modeling of gas diffusion loss contributions within the co-fired cell structure. This exemplifies how correlative tomography helps to understand specific contributions to overall cell performance

Design and Simulation of a Miniature Cylindrical Mirror Auger Electron Energy Analyzer with Secondary Electron Noise Suppression

In the nanoscale metrology industry, there is a need for low-cost instruments, which have the ability to probe the structrure and elemental composition of thin films. This dissertation, describes the research performed to design and simulate a miniature Cylindrical Mirror Analyzer, (CMA), and Auger Electron Spectrometer, (AES). The CMA includes an integrated coaxial thermionic electron source. Electron optics simulations were performed using the Finite Element Method, (FEM), software COMSOL. To address the large Secondary Electron, (SE), noise, inherent in AES spectra, this research also included experiments to create structures in materials, which were intended to suppress SE backgound noise in the CMA. Laser Beam Machining, (LBM), of copper substrates was used to create copper pillars with very high surface areas, which were designed to supress SE’s. The LBM was performed with a Lumera SUPER RAPID‐HE model Neodymium Vanadate laser. The laser has a peak output power of 30 megawatts, has a 5x lens and a spot size of 16 μm. The laser wavelength is in the infrared at 1064 nm, a pulse width of 15 picoseconds, and pulse repetition rate up to 100 kHz. The spectrometer used in this research is intended for use when performing chemical analysis of the surface of bulk materials and thin films. It is applicable for metrology of thin films, as low as 0.4 nm in thickness, without the need to perform destructive sample thinning, which is required in Scanning Tranmission Electron Microscopy, (STEM). The spectrometer design is based on the well known and widely used coaxial cylinder capacitor design known as the Cylindrical Mirror Analyzer, (CMA). The coaxial tube arrangement of the CMA allows for placing an electron source,which is mounted in the center of the inner cylinder of the spectrometer. Simulation of the electron source with an Einzel Lens was also performed. In addtion, experiments with thin film coatings and Laser Beam Machining to supress Secondary Electron emission noise within the Auger electron spectrum were completed. Design geometry for the miniature CMA were modeled using Computer Aided Design, (CAD). Fixed Boundary Conditions, (BC), were applied and the geometry was then meshed for FEM. The electrostatic potential was then solved using the Poisson equation at each point. Having found the solution to the electrostatic potentials, electron flight simulations were performed and compared with the analytical solution. From several commercially available FEM modeling packages, COMSOL Multiphysics was chosen as the research platform for modeling of the spectrometer design. The CMA in this design was reduced in size by a factor of 4 to 5. This enabled mounting the CMA on a 2 ¾ in flange compared to the commercial PHI model 660 CMA which mounts onto a 10 in flange. Results from the Scanning Electron Microscopy measurements of the Secondary Electron emission characteristics of the LBM electron suppressor will also be presented

Substrate interaction mediated control of phase separation in FIB milled Ag-Cu thin films

Nanofabrication is an integral part of realization of advanced functional devices ranging from optical displays to memory devices. Focused ion beam (FIB) milling is one of the widely used nanofabrication methods. Conventionally, FIB milling has been carried out for patterning single-phase stable thin films. However, the influence of FIB milling on phase separation of metastable alloy films during subsequent treatments has not been reported. Here, we show how FIB milling of Ag-Cu thin films influences the separation process and microstructure formation during post-milling annealing. Phase-separated microstructure of the film consists of fine, randomly distributed Ag-rich and Cu-rich domains, whereas adjacent to milled apertures (cylindrical holes), we observe two distinctly coarser rings. A combination of imaging and analysis techniques reveals Cu-rich islands dispersed in Ag-rich domains in the first ring next to the aperture, while the second ring constitutes mostly of Ag-rich grains. Copper silicide is observed to form in and around apertures through reaction with the Si-substrate. This substrate interaction, in addition to known variables like composition, temperature, and capillarity, appears to be a key element in drastically changing the local microstructure around apertures. This current study introduces new avenues to locally modulate the composition and microstructure through an appropriate choice of the film-substrate system. Such an ability can be exploited further to tune device functionalities with possible applications in plasmonics, catalysis, microelectronics and magnetics

The Boston University Photonics Center annual report 2013-2014

This repository item contains an annual report that summarizes activities of the Boston University Photonics Center in the 2013-2014 academic year. The report provides quantitative and descriptive information regarding photonics programs in education, interdisciplinary research, business innovation, and technology development. The Boston University Photonics Center (BUPC) is an interdisciplinary hub for education, research, scholarship, innovation, and technology development associated with practical uses of light.This annual report summarizes activities of the Boston University Photonics Center in the 2013–2014 academic year.This has been a good year for the Photonics Center. In the following pages, you will see that the center’s faculty received prodigious honors and awards, generated more than 100 notable scholarly publications in the leading journals in our field, and attracted $14.5M in new research grants and contracts this year. Faculty and staff also expanded their efforts in education and training, through National Science Foundation–sponsored sites for Research Experiences for Undergraduates and for Teachers. As a community, we hosted a compelling series of distinguished invited speakers, and emphasized the theme of Innovations at the Intersections of Micro/Nanofabrication Technology, Biology, and Biomedicine at our annual Future of Light Symposium. We took a leadership role in running national workshops on emerging photonic fields, including an OSA Incubator on Controlled Light Propagation through Complex Media, and an NSF Workshop on Noninvasive Imaging of Brain Function. Highlights of our research achievements for the year include a distinctive Presidential Early Career Award for Scientists and Engineers (PECASE) for Assistant Professor Xue Han, an ambitious new DoD-sponsored grant for Multi-Scale Multi-Disciplinary Modeling of Electronic Materials led by Professor Enrico Bellotti, launch of our NIH-sponsored Center for Innovation in Point of Care Technologies for the Future of Cancer Care led by Professor Cathy Klapperich, and successful completion of the ambitious IARPA-funded contract for Next Generation Solid Immersion Microscopy for Fault Isolation in Back-Side Circuit Analysis led by Professor Bennett Goldberg. These three programs, which represent more than$20M in research funding for the University, are indicative of the breadth of Photonics Center research interests: from fundamental modeling of optoelectronic materials to practical development of cancer diagnostics, from exciting new discoveries in optogenetics for understanding brain function to the achievement of world-record resolution in semiconductor circuit microscopy. Our community welcomed an auspicious cohort of new faculty members, including a newly hired assistant professor and a newly hired professor (and Chair of the Mechanical Engineering Department). The Industry/University Cooperative Research Center—the centerpiece of our translational biophotonics program—continues to focus on advancing the health care and medical device industries, and has entered its fourth year of operation with a strong record of achievement and with the support of an enthusiastic industrial membership base

Micromechanistic study of hydrogen embrittlement in pipeline steels

Hydrogen embrittlement, which causes the premature failure of steel pipelines, poses a long-standing challenge to hydrogen energy utilization. Ferrite-pearlite steels dominate the in-service hydrogen pipelines market. Yet hydrogen embrittlement mechanisms for the highly susceptible pearlite phase have remained inconclusive since the complicated microstructures in the bulk ferrite-pearlite steels interfere with categorizing the contribution of pearlite to hydrogen-induced failure. Here we provide a protocol combining in-situ micromechanical testing and ex-situ electrochemical hydrogen charging to successfully examine the effects of hydrogen on the mechanical behavior of pearlite and ferrite micropillars. In this project atom probe tomography with cryogenic-transfer technique was conducted on hydrogen-charged pearlite samples and observed hydrogen is trapped in the cementite lamellae rather than at the ferrite-cementite interfaces. The introduction of hydrogen reduces the yield strength of pearlite micropillars to a narrow range, which means that hydrogen weakens the anisotropic yielding of pearlite. Slip occurs at the ferrite-cementite interface for uncharged micropillars with inclined lamellae but after hydrogen charging it takes place in the ferrite matrix. Shear deformation dominates in micropillars with vertical and horizontal lamellae, where fracture occurs in the presence of hydrogen. Unlike pearlite, hydrogen only slightly reduces the yield strength of ferrite but has a greater impact on plasticity. Hydrogen softens ferrite micropillars and weakens intermittency during plastic deformation. These phenomena are attributed mainly to the hydrogen-enhanced local plasticity mechanism. This thesis also provides a new scanning electron microscope-based protocol to test the effect of hydrogen on the mechanical behavior of ferrite-pearlite steels that can facilitate fundamental studies on the interactions between hydrogen, microstructure, and deformation behavior

The Boston University Photonics Center annual report 2013-2014

This repository item contains an annual report that summarizes activities of the Boston University Photonics Center in the 2013-2014 academic year. The report provides quantitative and descriptive information regarding photonics programs in education, interdisciplinary research, business innovation, and technology development. The Boston University Photonics Center (BUPC) is an interdisciplinary hub for education, research, scholarship, innovation, and technology development associated with practical uses of light.This annual report summarizes activities of the Boston University Photonics Center in the 2013–2014 academic year.This has been a good year for the Photonics Center. In the following pages, you will see that the center’s faculty received prodigious honors and awards, generated more than 100 notable scholarly publications in the leading journals in our field, and attracted $14.5M in new research grants and contracts this year. Faculty and staff also expanded their efforts in education and training, through National Science Foundation–sponsored sites for Research Experiences for Undergraduates and for Teachers. As a community, we hosted a compelling series of distinguished invited speakers, and emphasized the theme of Innovations at the Intersections of Micro/Nanofabrication Technology, Biology, and Biomedicine at our annual Future of Light Symposium. We took a leadership role in running national workshops on emerging photonic fields, including an OSA Incubator on Controlled Light Propagation through Complex Media, and an NSF Workshop on Noninvasive Imaging of Brain Function. Highlights of our research achievements for the year include a distinctive Presidential Early Career Award for Scientists and Engineers (PECASE) for Assistant Professor Xue Han, an ambitious new DoD-sponsored grant for Multi-Scale Multi-Disciplinary Modeling of Electronic Materials led by Professor Enrico Bellotti, launch of our NIH-sponsored Center for Innovation in Point of Care Technologies for the Future of Cancer Care led by Professor Cathy Klapperich, and successful completion of the ambitious IARPA-funded contract for Next Generation Solid Immersion Microscopy for Fault Isolation in Back-Side Circuit Analysis led by Professor Bennett Goldberg. These three programs, which represent more than$20M in research funding for the University, are indicative of the breadth of Photonics Center research interests: from fundamental modeling of optoelectronic materials to practical development of cancer diagnostics, from exciting new discoveries in optogenetics for understanding brain function to the achievement of world-record resolution in semiconductor circuit microscopy. Our community welcomed an auspicious cohort of new faculty members, including a newly hired assistant professor and a newly hired professor (and Chair of the Mechanical Engineering Department). The Industry/University Cooperative Research Center—the centerpiece of our translational biophotonics program—continues to focus on advancing the health care and medical device industries, and has entered its fourth year of operation with a strong record of achievement and with the support of an enthusiastic industrial membership base