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At least 469 records · Page 26

High Resolution Transmission Electron Microscopy (HRTEM) of nanophase ferric oxides

Iron oxide minerals are the prime candidates for Fe(III) signatures in remotely sensed Martian surface spectra. Magnetic, Mossbauer, and reflectance spectroscopy have been carried out in the laboratory in order to understand the mineralogical nature of Martian analog ferric oxide minerals of submicron or nanometer size range. Out of the iron oxide minerals studied, nanometer sized ferric oxides are promising candidates for possible Martian spectral analogs. 'Nanophase ferric oxide (np-Ox)' is a generic term for ferric oxide/oxihydroxide particles having nanoscale (less than 10 nm) particle dimensions. Ferrihydrite, superparamagnetic particles of hematite, maghemite and goethite, and nanometer sized particles of inherently paramagnetic lepidocrocite are all examples of nanophase ferric oxides. np-Ox particles in general do not give X-ray diffraction (XRD) patterns with well defined peaks and would often be classified as X-ray amorphous. Therefore, different np-Oxs preparations should be characterized using a more sensitive technique e.g., high resolution transmission electron microscopy (HRTEM). The purpose of this study is to report the particle size, morphology and crystalline order, of five np-Ox samples by HRTEM imaging and electron diffraction (ED).

Golden, D. C.↗

Investigation of nucleation and growth processes of diamond films by atomic force microscopy

The nucleation and growth of plasma-enhanced chemical-vapor deposited polycrystalline diamond films were studied using atomic force microscopy (AFM). AFM images were obtained for (1) nucleated diamond films produced from depositions that were terminated during the initial stages of growth, (2) the silicon substrate-diamond film interface side of diamond films (1-4 micrometers thick) removed from the original surface of the substrate, and (3) the cross-sectional fracture surface of the film, including the Si/diamond interface. Pronounced tip effects were observed for early-stage diamond nucleation attributed to tip convolution in the AFM images. AFM images of the film's cross section and interface, however, were not highly affected by tip convolution, and the images indicate that the surface of the silicon substrate is initially covered by a small grained polycrystalline-like film and the formation of this precursor film is followed by nucleation of the diamond film on top of this layer. X-ray photoelectron spectroscopy spectra indicate that some silicon carbide is present in the precursor layer.

George, M. A.↗

Scanning electron acoustic microscopy of residual stresses in ceramics: Theory and experiment

Several reviews have highlighted a number of applications of scanning electron acoustic microscopy (SEAM) to metals and semiconductors which show that SEAM can provide new information on surface and near-surface features of such materials, but there have been few studies attempting to determine the capabilities of SEAM for characterizing ceramic materials. We have recently observed image contrast in SEAM from residual stress fields induced in brittle materials by Vickers indentations that is strongly dependent on the electron beam chopping frequency. We have also recently developed a three-dimensional mathematical model of signal generation and contrast in SEAM, appropriate to the brittle materials studied, that we use as a starting point in this paper for modeling the effect of residual stress fields on the generated electron acoustic signal. The influence of the electron beam chopping frequency is also considered under restrictive assumptions.

Cantrell, John H.↗

Investigation of nucleation and growth processes of diamond films by atomic force microscopy

The nucleation and growth of plasma enhanced chemical vapor deposited (PECVD) polycrystalline diamond films were studied using atomic force microscopy (AFM). AFM images were obtained for: (1) nucleated diamond films produced from depositions that were terminated during the initial stages of growth, (2) the silicon substrate-diamond film interface side of diamond films (1-4 micrometers thick) removed from the original surface of the substrate, and (3) cross-sectional fracture surface of the film, including the Si/diamond interface. Pronounced tip effects were observed for early-stage diamond nucleation attributed to tip convolution in the AFM images. AFM images of the films cross-section and interface however were not affected by tip convolution, and the images indicate that the surface of the silicon substrate is initially covered by small grained polycrystalline-like film and the formation of this precursor film is followed by nucleation of the diamond film on top of this layer. X-ray photoelectron spectroscoy (XPS) spectra indicates that some silicon carbide is present in the precursor layer.

George, M. A.↗

Scanning Tunneling Microscopy Studies of Diamond Films and Optoelectronic Materials

We present a summary of the research, citations of publications resulting from the research and abstracts of such publications. We have made no inventions in the performance of the work in this project. The main goals of the project were to set up a Chemical Vapor Deposition (CVD) diamond growth system attached to an UltraHigh Vacuum (UHV) atomic resolution Scanning Tunneling Microscopy (STM) system and carry out experiments aimed at studying the properties and growth of diamond films using atomic resolution UHV STM. We successfully achieved these goals. We observed, for the first time, the atomic structure of the surface of CVD grown epitaxial diamond (100) films using UHV STM. We studied the effects of atomic hydrogen on the CVD diamond growth process. We studied the electronic properties of the diamond (100) (2x1) surface, and the effect of alkali metal adsorbates such as Cs on the work function of this surface using UHV STM spectroscopy techniques. We also studied, using STM, new electronic materials such as carbon nanotubes and gold nanostructures. This work resulted in four publications in refereed scientific journals and five publications in refereed conference proceedings.

Perez, Jose M.↗

Advancement of X-Ray Microscopy Technology and its Application to Metal Solidification Studies

The technique of x-ray projection microscopy is being used to view, in real time, the structures and dynamics of the solid-liquid interface during solidification. By employing a hard x-ray source with sub-micron dimensions, resolutions of 2 micrometers can be obtained with magnifications of over 800 X. Specimen growth conditions need to be optimized and the best imaging technologies applied to maintain x-ray image resolution, contrast and sensitivity. It turns out that no single imaging technology offers the best solution and traditional methods like radiographic film cannot be used due to specimen motion (solidification). In addition, a special furnace design is required to permit controlled growth conditions and still offer maximum resolution and image contrast.

Kaukler, William F.↗

Ballistic-Electron-Emission-Microscopy of Strained Si(sub 1-x)Ge(sub x) Layers

Ballistic-electron-emission microscopy (BEEM) has been used to investigate the effects of strain on Si(sub 1-x)Ge(sub x) alloys. Lifting of the degeneracy of the conduction-band minimum of Si(sub 1-x)Ge(sub x), due to lattice deformation has been directly measured by application of BEEM spectroscopy to Ag/Si structures. Experimental values for this conduction-band splitting agree well with calculations. In addition, an unexpected heterogeneity in the strain of the Si(sub 1-x)Ge(sub x) layer is introduced by deposition of Au. This effect, not observed with Ag, is attributed to species interdiffusion and has important implications for metal-semiconductor devices based oil pseudomorphic Si(sub 1-x)Ge(sub x)/Si material systems.

Bell, L. D.↗

Advancement of X-Ray Microscopy Technology and Its Application to Metal Solidification Studies

The technique of x-ray projection microscopy is being used to view, in real time, the structures and dynamics of the solid-liquid interface during solidification. By employing a hard x-ray source with sub-micron dimensions, resolutions of 2 microns can be obtained with magnifications of over 800 X. Specimen growth conditions need to be optimized and the best imaging technologies applied to maintain x-ray image resolution, contrast and sensitivity. It turns out that no single imaging technology offers the best solution and traditional methods like radiographic film cannot be used due to specimen motion (solidification). In addition, a special furnace design is required to permit controlled growth conditions and still offer maximum resolution and image contrast.

Kaukler, William F.↗

Evidence of Momentum Conservation at a Nonepitaxial Metal/Semiconductor Interface Using Ballistic Electron Emission Microscopy

Ballistic-Electron-Emission Microscopy (BEEM) spectroscopy has been performed on Au/Si(111) structures as a function of Au thickness and temperature. At 77 K a direct signature of parallel momentum conservation at the Au/Si interface is observed in the BEEM spectra. The variation in spectral shape with both Au thickness and temperature places restrictions on allowable values of inelastic and elastic mean-free paths in the metal, and also requires the presence of multiple electron passes within the Au layer. An independent indication of multiple reflections is directly observed in the attenuation of BEEM current with Au thickness.

Bell, L. D.↗

Real-Time X-Ray Transmission Microscopy for Fundamental Studies Solidification

High resolution real-time X-ray Transmission Microscopy, XTM, has been applied to obtain information fundamental to solidification of optically opaque metallic systems. We have previously reported the measurement of solute profile in the liquid, phase growth, and detailed solid-liquid interfacial morphology of aluminum based alloys with exposure times less than 2 seconds. Recent advances in XTM furnace design have provided an increase in real-time magnification (during solidification) for the XTM from 4OX to 16OX. The increased magnification has enabled for the first time the XTM imaging of real-time growth of fibers and particles with diameters of 5 micrometers. We have applied this system to study of the kinetics of formation and morphological evolution of secondary fibers and particles in Al-Bi monotectic alloys to observe a previously unreported velocity dependent thermo-capillary depletion mechanism for Bi rich liquid which can penetrate many fiber diameters into the solid-liquid interface. In this talk we will discuss application of the XTM to the study the fundamentals of monotectic and eutectic solidification, the enhancement of XTM data with precise solid liquid interfacial temperature and thermal gradient measurement techniques, and the application of this technology to the study of the fundamentals of solidification in microgravity,

Curreri, Peter A.↗

Chemical Silver Coating of Fiber Tips in Near-Field Scanning Optical Microscopy

We report what is believed to be the first experimental demonstration of silver coating by a wet chemical process on tapered fiber tips used in near-field scanning optical microscopy. The process is at room temperature and pressure and takes only a few minutes to complete. Many tips can be simultaneously coated.

Vikram, Chandra S.↗

Determining the Molecular Packing Arrangements on Protein Crystal Faces by Atomic Force Microscopy

Periodic Bond Chain (PBC) analysis of the packing of tetragonal lysozyme crystals have revealed that there are two possible molecular packing arrangements for the crystal faces. The analysis also predicted that only one of these, involving the formation of helices about the 4(sub 3) axes, would prevail during crystal growth. In this study high resolution atomic force microscopy (AFM) was employed to verify these predictions for the (110) crystal face. A computer program was developed which constructs the expected AFM image for a given tip shape for each possible molecular packing arrangement. By comparing the actual AFM image with the predicted images the correct packing arrangement was determined. The prediction of an arrangement involving 4(sub 3) helices was confirmed in this manner,"while the alternate arrangement was not observed. The investigation also showed the protein molecules were packed slightly closer about the 4(sub 3) axes than in the crystallographic arrangement of the crystal interior. This study demonstrates a new approach for determining the molecular packing arrangements on protein crystal faces. It also shows the power of combining a theoretical PBC analysis with experimental high resolution AFM techniques in probing protein crystal growth processes at the molecular level.

Li, Huayu↗

Determining the Molecular Growth Mechanisms of Protein Crystal Faces by Atomic Force Microscopy

A high resolution atomic force microscopy (AFM) study had shown that the molecular packing on the tetragonal lysozyme (110) face corresponded to only one of two possible packing arrangements, suggesting that growth layers on this face were of bimolecular height. Theoretical analyses of the packing also indicated that growth of this face should proceed by the addition of growth units of at least tetramer size corresponding to the 43 helices in the crystal. In this study an AFM linescan technique was devised to measure the dimensions of individual growth units on protein crystal faces as they were being incorporated into the lattice. Images of individual growth events on the (110) face of tetragonal lysozyme crystals were observed, shown by jump discontinuities in the growth step in the linescan images as shown in the figure. The growth unit dimension in the scanned direction was obtained from these images. A large number of scans in two directions on the (110) face were performed and the distribution of lysozyme growth unit sizes were obtained. A variety of unit sizes corresponding to 43 helices, were shown to participate in the growth process, with the 43 tetramer being the minimum observed size. This technique represents a new application for AFM allowing time resolved studies of molecular process to be carried out.

Nadarajah, Arunan↗

Observation of Individual Fluorine Atom from Highly Oriented Poly (tetrafluoroethylene) Films by Atomic Force Microscopy

Direct observation of the film thickness, molecular structure and individual fluorine atoms from highly oriented poly(tetrafluoroethylene) (PTFE) films were achieved using atomic force microscopy (AFM). A thin PTFE film is mechanically deposited onto a smooth glass substrate at specific temperatures by a friction transfer technique. Atomic resolution images of these films show that the chain-like helical structures of the PTFE macromolecules are aligned parallel to each other with an intermolecular spacing of 5.72 A, and individual fluorine atoms are clearly observed along these twisted molecular chains with an interatomic spacing of 2.75 A. Furthermore, the first direct AFM measurements for the radius of the fluorine-helix, and of the carbon-helix in sub-angstrom scale are reported as 1.70 A and 0.54 A respectively.

Lee, Jonathan A.,↗

Determining the Molecular Growth Mechanisms of Protein Crystal faces by Atomic Force Microscopy

A high resolution atomic force microscopy (AFM) study had shown that the molecular packing on the tetragonal lysozyme (110) face corresponded to only one of two possible packing arrangements, suggesting that growth layers on this face were of bimolecular height (Li et al., 1998). Theoretical analyses of the packing had also indicated that growth of this face should proceed by the addition of growth units of at least tetramer size corresponding to the 43 helices in the crystal. In this study an AFM linescan technique was devised to measure the dimensions of individual growth units on protein crystal faces. The growth process of tetragonal lysozyme crystals was slowed down by employing very low supersaturations. As a result images of individual growth events on the (110) face were observed, shown by jump discontinuities in the growth step in the linescan images. The growth unit dimension in the scanned direction was obtained by suitably averaging these images. A large number of scans in two directions on the (110) face were performed and the distribution of lysozyme aggregate sizes were obtained. A variety of growth units, all of which were 43 helical lysozyme aggregates, were shown to participate in the growth process with a 43 tetramer being the minimum observed size. This technique represents a new application for AFM allowing time resolved studies of molecular process to be carried out.

Li, Huayu↗

Near-Field Scanning Optical Microscopy of Soft, Biological, or Rough Objects in Aqueous Environment: Challenges and some Remedies to Circumvent

Near-field scanning optical microscopy is an established technique for sub-wavelength spatial resolution in imaging, spectroscopy, material science, surface chemistry, polarimetry, etc. A significant amount of confidence has been established for thin hard specimens in air. However when soft, biological, rough, in aqueous environment object, or a combination is involved, the progress has been slow. The tip-sample mechanical interaction, heat effects to sample, drag effects to the probe, difficulty in controlling tip-sample separation in case of rough objects, light scattering from sample thickness, etc. create problems. Although these problems are not even fully understood, there have been attempts to study them with the aim of performing reliable operations. In this review we describe these attempts. Starting with general problems encountered, various effects like polarization, thermal, and media are covered. The roles of independent tip-sample distance control tools in the relevant situations are then described. Finally progress in fluid cell aspect has been summarized.

Vikram, C. S.↗

Observation of Individual Fluorine Atoms from Highly Oriented Poly(Tetrafluoroethylene) Films by Atomic Force Microscopy

Direct observation of the film thickness, molecular structure, and individual fluorine atoms from highly oriented poly(tetrafluoroethylene) (PTFE) films were achieved using atomic force microscopy (AFM). A thin PTFE film is mechanically deposited onto a smooth glass substrate at specific temperatures by a friction-transfer technique. Atomic resolution images of these films show that the chain-like helical structures of the PTFE macromolecules are aligned parallel to each other with an intermolecular spacing of 5.72 A, and individual fluorine atoms are clearly observed along these twisted molecular chains with an interatomic spacing of 2.75 A. Furthermore, the first direct AFM measurements for the radius of the fluorine-helix, and of the carbon-helix in sub-angstrom scale are reported as 1.7 and 0.54 A respectively.

Lee, J. A.↗

Fabrication and Atomic Force Microscopy Characterization of Molecular Composites of Fullerenes in Aerogel Matrix for Optical Limiting

An optical limiter is a device which exhibits a decrease in the transmittance in a material with an increase in intensity of light. Sol-gel techniques offer many advantages in the fabrication of materials. These materials possess many desirable properties for nonlinear optical (NLO) device applications which include transparency, high thermal and chemical stabilities, very low refractive index and dielectric constants. C60 shows a higher excited state absorption cross section than the ground state absorption cross section over the complete visible spectrum, and the spectrum of the excited state absorption of C60 has the same general shape as the ground state absorption. This fact suggests that fullerenes are ideal optical limiting materials. Aerogels are fabricated by sol-gel processing. One of the key issues is the dispersion of fullerenes into small and uniform pores of silica aerogel host matrices. The aerogel network was characterized by Raman spectroscopy. Atomic force microscopy is a technique with many advantages to characterize the aerogel materials. The morphology of the cleaved surface for a C60/aerogel sample shows that there are long paralleled shaped stripes with 20-30 nm in width and about 500 nm in length on the cleaved surface. The cleaved surface also was etched by 5% HF solution for one minutes, and it became smoother after HF etching. The main feature in on the surface is the spherical particles with the size of few nanometers, and no aggregated fullerenes appear. The fullerenes are well dispersed in the aerogel matrices.

Lu, W. J .↗