Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

Pseudomorphic HEMT (p-HEMT) devices are used in a number of wireless communication applications including power amplifiers in the 17–50 GHz range, low noise amplifiers and switches. Selective wet etching is often used to form the gate regions of these devices to avoid plasma damage associated with dry etching. We have investigated the wet etching of small (8μm to 0.5μm) features with organic acid - hydrogen peroxide solutions. Two acid solutions were used as a selective etchant for GaAs using AlAs etch stop layers in a p-HEMT structure grown by MBE. The etched features were characterized by AFM, SEM, and TEM techniques. The etch depth uniformity and reproducibility were found to depend on a number of factors including feature size, feature density, etching chemistry, agitation and surface tension. When features with a range of size and density were placed in close proximity in a layout we found that the etch rate of the different features was a function of density, size and most importantly the etch chemistry. One etchant solution exhibited a 12% difference in etch rate from the smallest feature to the largest, while another solution exhibited uniform etching of all features regardless of size or density. Both solutions produced specular etched surfaces in GaAs and AlGaAs. However, the AlAs etch stop showed a non-uniform surface morphology after etching. The surface morphology of the AlAs etch stop is one factor that limits the over etch which can be designed into the process. The most important factors to be considered in designing a selective etch process will be presented.

Electrospinning of polycarbonate with solvent mixtures of THF (Tetrahydrofuran) and DMF (Dimethylformamide) has been performed. The effect of various process parameters like voltage, concentration, flow rate and distance has been investigated to yield uniform polycarbonate nanofibers with minimal bead densities. The temperature and humidity have also been carefully monitored for all the runs. The Design of Experiment (DOE) has been conducted with the help of Minitab software to find the most significant parameter for obtaining uniform beadless nanofibers. These uniform nanofibers can then be used in future work to produce TiO2 nanotubes.

Aluminum silicate nanoaggregates grown on organic multilayer templates were imaged by a transmission electron microscope. Images were processed by fractal and FOURIER analysis. The estimated mass fractal dimension suggested that aggregate formation was diffusion limited. Nonlinear filtering of FOURIER spectra, which included comparison with a model spectral density, yielded «enhanced power spectra». Some morphological descriptors were extracted from the latter. The main result, materials classification, was attained by a two-scale procedure. Some descriptors were related to the material properties such as nanoparticle size distribution and sharpness of aggregate boundaries.

Electrically conducting organic polymers are a novel class of ‘synthetic metals’ that combine the chemical and mechanical properties of polymers with the electronic properties of metals and semiconductors. Electronically conducting polymers have been studied extensively owing to their applications in energy conversion devices, sensors, electro chromic devices, electromagnetic interference shielding (EMI), electronic circuits etc. Polyaniline - an organic conducting polymer - has been blended with poly methyl methacrylate and the blends have been electrospun to produce conducting nanofibers. The electrospun blends have been characterized to study fiber morphology and formulate conditions for nanofiber formation.

Electrospinning is a superior process compared to other conventional spinning methods for the production of fibers in the sub-micron to nanometer scales. Such fiber membranes have exceptionally large surface areas and small pore sizes. The process requires an electrostatic force, which induces charges on the liquid droplet of the polymer solution or melts and therefore overcomes the surface tension and viscoelasticity forces to create an electrically charged jet. When the jet dries or solidifies, an electrically charged fiber remains, which can be directed or accelerated by the electrical forces and then collected in non-woven fiber membrane or other useful shapes. The present research work demonstrates the electrospinning of polycarbonate solution with solvent mixtures THF (Tetrahydrofuran) and DMF (Di-methyl formamide) to produce nanometer scale polycarbonate fibers. The solvent mixture of THF and DMF was the major parameter for producing nano-polycarbonate fibers along with the formation of byproducts beads. The electrostatic voltage, viscosity and surface tension also showed significant effect on bead formation and bead density. The microstructures of the polycarbonate beads were quantitvely investigated by Scanning Electron Microscope (SEM) and Transmission Electron Microscope (TEM).

Ever since the discovery of the astonishing properties of GaN, many research groups have been involved in the processing of the perfect GaN crystal. Iodine Vapor Phase Growth (IVPG) technique was employed to grow GaN epilayer on a MOCVD pre-deposited buffer layer. This new epitaxial system was characterized by TEM, AFM and EFM. A complete AFM study involved the polarity measurements and the etch pit density measurements. For the first time a systematic study was performed of the dislocation density changing as a function of distance from the substrate. TEM performed on the cross-section, as well as the plan view, of the samples showed a remarkable decrease in the dislocations in the current system, compared to the samples that were solely deposited by MOCVD. Advanced analytical methods of polarity and dislocation density measurements have been established to understand the relation between microstructure and electrical properties of the thick film GaN. Electrostatic Force Microscopy has been suggested as a potential tool for obtaining polarity information.

Unlike conventional spin methods, electrospinning is capable of yielding fibers with sub-micron range diameters and high specific surface areas. The use of such electrospun materials in applications, whose functionality depends on the area available, such as separation processes, will be useful. In this study a Bisphenol-A polycarbonate was dissolved in two solvents: Chloroform and a 1:1 mixture of Tetrahydrofuran (THF) and Dimethylformamide (DMF) and resulting polycarbonate solutions were then electrospun to produce polycarbonate fiber-mats. The morphological features of the electrospun polycarbonate fibers have been studied as a function of the solvent used and also as a function of the processing voltage. The studies were conducted using the SEM, TEM and Scion image analysis program. The results indicate bold differences in the fiber morphology and bead density trends with the solvent used. Electrospun polycarbonate fibers exhibit a “Raisin like” puckered structure. Such a structure will enhance the functional efficiency of an electrospun material when used in an area-based application. In addition, studies on crazing of bulk polycarbonate and the surface features of electrospun polycarbonate fibers have been conducted. Results indicate a relation between crazing and the topological features of electrospun polycarbonates.

Multilayer nanocomposite films have been prepared from exfoliated aluminosilicate/coumarin dye complex through layer-by-layer self-assembly using cationic polyelectrolytes. Coumarin dye molecules were intercalated into the layered aluminosilicate by an ion exchange reaction. Particles of the hectorite/dye complex were delaminated by extensive shaking and sonication of their water suspension into 2∼3 nm-thin silicate layers with molecules of the dye adsorbed on their surface. Atomic force microscopy and transmission electron microscopy data are in agreement with such a model. Ultrathin multilayered films were prepared using layer-by-layer self-assembly from the aluminosilicate platelets and a cationic polyelectrolyte polydiallyldimethylammonium chloride (PDAC). Linear build-up of the films up to 20 cycles was demonstrated and investigated using absorption spectroscopy and spectrofluorometer. The resulting transparent films have exhibited strong characteristic blue-green fluorescence due to coumarin dye molecules adhered to the exfoliated hectorite platelets.

The precipitates in nitrogen-added type 316L stainless steels (SS) were investigated by transmission electron microscopy (TEM) after thermal aging. Besides carbides (M23C6 and M6C) and intermetallic phases, an unknown phase of an Fe–Mo–Cr(–Si) system n a filmlike morphology precipitated at grain boundaries. In spite of the similarity in ts chemical composition to that of the Laves phase, the phase of the Fe–Mo–Cr(–Si) system exhibited five-, three-, and twofold symmetries, which are generally observed in quasicrystals having icosahedral symmetry. This phase was formed from the intergrowth of small crystalline clusters of the Laves phase. Decreasing the nitrogen content to that of commercial type 316L grade suppressed the formation of the filmlike fivefold phase. This was attributed to the dissipation of small Laves clusters by M23C6 carbides, which increased as a result of the decreased nitrogen content.

This work is focused on dust or debris produced by the wear of tire tread. Two problems are addressed, which are solved by analytical electron microscopy (AEM): characterization of tire debris and identification of tire debris particles in a heterogeneous specimen. The characteristic morphology, microstructure and elemental composition of tire debris can all be determined by AEM. The scanning electron microscope (SEM) shows that the surface of a tire debris particle has a typical, warped structure with pores. The characteristic elements of tire rubber are S and Zn, which are detected by energy dispersive X ray (EDX) spectroscopy. The identification of rubber particles in heterogeneous debris containing talc and produced by a laboratory abrader is possible by the analytical SEM. Transmission electron microscope images, EDX spectra and selected area electron diffraction patterns characterize tire debris at the sub–micron scale, where the material can no longer be treated as homogeneous.

Because of their high coercivity, cobalt alloy thin films are among the most popular materials used for ultra-high density longitudinal magnetic recording media. The recording and magnetic properties of the materials are related to their microstructure; in particular, depletion of Co in a grain boundary phase, and physical separation of the grains act to increase coercivity and thus to produce low noise media. We are studying a new alloy system comprising 18 nm thick Co-Cr-P-Pt films (Mr.t ≈ 0.9 memu/cm2), prepared by DC sputtering. A coercivity of 2600 Oe or higher was obtained in these films even when they were deposited without heating the substrate or applying a bias voltage. The effects of P and Pt addition were characterized by high-resolution TEM coupled with energy dispersive x-ray spectroscopy (EDS) and electron energy loss spectroscopy (EELS). A Hitachi HF-2000 field emission TEM was used to image both low P (≈ 6 at. %) and high P (≈ 12 at. %) samples, and to provide a 1 nm beam for high spatial resolution EDS and EELS.

Cubic boron nitride films were prepared by helicon wave plasma CVD process on (100) Si. The film deposited under the intense impact of energetic ions is usually delaminated from the substrate after deposition. The delamination behavior of c-BN film was investigated with transmission electron microscopy. It is found that moisture in the air, surface roughness of the film and substrate, as well as severe compressive stresses in the film are the primary contributors to film delamination. An aqueous oxidation was verified by EDXS analysis, which generate local stress by volume expansion at the crack region in the c-BN layer.

The cross-sectional TEM micrograph of c-BN film in Fig. 1 shows that a very thin layer of h-BN is deposited before the c-BN layer starts to grow at an early stage of film growth. A columnar structured thin h-BN layer about 20 nm thickness at the interface is clearly separated from the c-BN layer in an aspect of microstructure.

Highly oriented diamond films were deposited on a (001) silicon substrate by bias enhanced MPCVD technique. Three-dimensional TEM characterizations were carried out to understand the nucleation and growth mechanism of diamond grains. The surface morphology, defects, and misorientations of diamond films were compared as a function of synthesizing temperatures and thickness of the films. From our experimental results the texture formation mechanism of diamond films is discussed.