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Nanoscale Subsurface Imaging of Nanocomposites via Resonant Difference-Frequency Atomic Force Ultrasonic Microscopy

A scanning probe microscope methodology, called resonant difference-frequency atomic force ultrasonic microscopy (RDF-AFUM), has been developed. The method employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope engages the sample top surface. The cantilever is driven at a frequency differing from the ultrasonic frequency by one of the contact resonance frequencies of the cantilever. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave at the sample surface generates difference-frequency oscillations at the cantilever contact resonance. The resonance-enhanced difference-frequency signals are used to create amplitude and phase-generated images of nanoscale near-surface and subsurface features. RDF-AFUM phase images of LaRC-CP2 polyimide polymer containing embedded nanostructures are presented. A RDF-AFUM micrograph of a 12.7 micrometer thick film of LaRC-CP2 containing a monolayer of gold nanoparticles embedded 7 micrometers below the specimen surface reveals the occurrence of contiguous amorphous and crystalline phases within the bulk of the polymer and a preferential growth of the crystalline phase in the vicinity of the gold nanoparticles. A RDF-AFUM micrograph of LaRC-CP2 film containing randomly dispersed carbon nanotubes reveals the growth of an interphase region at certain nanotube-polymer interfaces.

Cantrell, Sean A.

Investigating Variations in Water Abundances in Lunar Felsite Clasts Using Coordinated Field-Emission STEM and NanoSIMS Analyses

As representatives of petrochemically-evolved igneous rocks on the Moon, the granitic felsite clasts in lunar breccias have come under renewed focus as part of new efforts to use feldspars for assessing the inventory of lunar water and other volatiles. Previous petrologic studies of these clasts were tilted towards finding those assemblages and relationships most likely to be direct products of magmatic processes. In support of our on-going NanoSIMS (Nanoscale Secondary Ion Mass Spectrometry) measurements of trace water contents in the feldspars in these clasts, we are using coordinated analytical SEM (Scanning Electron Microscopy), electron probe microanalyzer (EPMA) and analytical field emission scanning transmission electron microscopy (FE-STEM) techniques to re-evaluate the full diversity of processes under which the feldspar-bearing assemblages in these clasts formed. Here we report a comparison of FE-STEM imaging and microanalysis results obtained on focused ion beam (FIB) sections extracted from felsite (alkali feldspar plus SiO2 plus or minus plagioclase) clasts in lunar breccias 15405 and 12013. The feldspars in these clasts have water contents which, although relatively low (7-18 ppm) by terrestrial standards, still show values significantly higher than measurements (approximately 0.5 ppm) of nominally anhydrous NanoSIMS standards.

Christoffersen, Roy

Virtual Prototyping for Carbon Nanotubes and Their Compositions

Carbon nanotubes (CNT) are of interest as constituents-reinforcements for composites, probes for scanning microscopy, quantum wires for electronics, and building blocks for nanomachinery. Their small size makes direct experimental measurements difficult. Therefore, the critical answers about their properties should be obtained based on adequate modeling, virtual prototyping, using the methods of classical molecular dynamic (MD), in combination with the analytical methods and continuum mechanics.

Yakobson, Boris I.

Carbon nanotubes and nanowires for biological sensing

This chapter reviews the recent development in biological sensing using nanotechnologies based on carbon nanotubes and various nanowires. These 1D materials have shown unique properties that are efficient in interacting with biomolecules of similar dimensions, i.e., on a nanometer scale. Various aspects including synthesis, materials properties, device fabrication, biofunctionalization, and biological sensing applications of such materials are reviewed. The potential of such integrated nanobiosensors in providing ultrahigh sensitivity, fast response, and high-degree multiplex detection, yet with minimum sample requirements is demonstrated. This chapter is intended to provide comprehensive updated information for people from a variety of backgrounds but with common interests in the fast-moving interdisciplinary field of nanobiotechnology.

Review

In-situ chemical imager

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in-situ instruments scanning probe microscopy lase

In-situ chemical imager

A variety of in-situ planetary exploration tasks such as particulate analysis or life detection require a tool with a capability for combined imaging and chemical analysis with sub-micron spatial resolution.

spectroscopy SPM LIBS

Nanoscale Subsurface Imaging via Resonant Difference-Frequency Atomic Force Ultrasonic Microscopy

A novel scanning probe microscope methodology has been developed that employs an ultrasonic wave launched from the bottom of a sample while the cantilever of an atomic force microscope, driven at a frequency differing from the ultrasonic frequency by the fundamental resonance frequency of the cantilever, engages the sample top surface. The nonlinear mixing of the oscillating cantilever and the ultrasonic wave in the region defined by the cantilever tip-sample surface interaction force generates difference-frequency oscillations at the cantilever fundamental resonance. The resonance-enhanced difference-frequency signals are used to create images of embedded nanoscale features.

Cantrell, Sean A.

Methods of analyzing microsize particulate aerosols and contaminants.

Methods for analyzing atmospheric aerosols and particulate contaminants from natural and industrial sources are briefly described. Their development was spurred by interest in cosmic dust investigations. These methods make it possible to analyze individual particles ranging in size from 0.01 to 1000 microns for elemental and mineralogical content. The described methods include transmission electron microscopy, scanning electron microscopy, electron probe microanalysis, X-ray diffraction, optical mineralogy, and density measurement.

Blanchard, M. B.

Structure and properties of solid surfaces

Difficulties in experimental studies of crystalline surfaces are related to the fact that surface atoms have an intrinsic tendency to react with their environment. A second problem is connected with the effective thickness of surfaces, which ranges from one to several atom layers. The phenomenology of surface interactions with gases are considered, taking into account physical adsorption, chemisorption, and the oxidation of surfaces. Studies of the surface structure are discussed, giving attention to field emission microscopy, field-ion microscopy, electron diffraction techniques, Auger spectroscopy, scanning electron microscopy, electron probe microanalysis, ion microprobe methods, and low-energy backscattering spectroscopy. Investigations of semiconductor surfaces are also described.

Gatos, H. C.

M551 metals melting experiment

Electron beam welding studies were conducted in the Skylab M551 metals melting experiment, on three different materials; namely 2219-T87 aluminum alloy, 304L stainless steel, and commercially pure tantalum (0.5 wt % columbium). Welds were made in both one gravity and zero gravity (Skylab) environments. Segments from each of the welds were investigated by microhardness, optical microscopy, scanning microscopy, and electron probe techniques. In the 2219-T87 aluminum alloy samples, macroscopic banding and the presence of an eutectic phase in the grain boundaries of the heat affected zone were observed. The stainless steel samples exhibited a sharp weld interface and macroscopic bands. The primary microstructural features found in the tantalum were the presence of either columnar grains (ground base) or equiaxed grains (Skylab). The factors contributing to these effects are discussed and the role of reduced gravity in welding is considered.

Busch, G.

Mechanical property degradation and chemical interactions in Borsic/titanium composite

A study was undertaken to identify the mechanisms of mechanical property degradation in a Borsic (silicon-carbide coated boron) fiber reinforced Ti-3Al-2.5V composite exposed to elevated temperature. Samples containing 0.45 volume fraction of fibers were exposed, in vacuum, to temperatures from 700 K to 1255 K for times up to 240 hours. Room temperature tensile properties of unidirectional material were determined in both the longitudinal and transverse directions, before and after high-temperature exposure. Electron micro-probe analysis, scanning electron microscopy, and X-ray diffraction were used to determine the compounds formed and the extent of interaction between the boron, SiC coating, and matrix materials.

Brewer, W. D.

Electron-optical observations of ordered FeNi in the Estherville meteorite

Electron optical studies of the ordered FeNi (taenite) phase in the Estherville meteorite are reported. A thin section of the meteorite containing a large area of continuous anisotropic taenite was studied by crossed polar reflected light microscopy, and electron probe microanalysis, transmission electron microscopy, scanning transmission electron microscopy and X-ray energy dispersive spectrometry. Results reveal the presence of preferentially ion-etched regions of clear taenite corresponding to single crystals, with superlattice reflections in the fundamental FeNi reciprocal lattice arising from long-range ordering. The presence of antiphase domain boundaries within the regions also confirms the presence of ordering. It is thus proposed that clear taenite in the Estherville meteorite contains regions of ordered FeNi phase in a disordered gamma-phase matrix.

Mehta, S.

Microstructural stability of wrought, laser and electron beam glazed NARloy-Z alloy at elevated temperatures

Microstructure of wrought, laser, and electron-beam glazed NARloy-Z(Cu-3 wt.% Ag-0.5 wt.% Zr) was investigated for thermal stability at elevated temperatures (539 to 760 C (1,100 to 1,400 F)) up to 94 h. Optical and scanning electron microscopy and electron probe microanalysis were employed for studying microstructural evolution and kinetics of precipitation. Grain boundary precipitation and precipitate free zones (PFZ's) were observed in the wrought alloy after exposing to temperatures above 605 C (1,120 F). The fine-grained microstructure observed in the laser and electron-beam glazed NARloy-Z was much more stable at elevated temperatures. Microstructural changes correlated well with hardness measurements.

Singh, J.

Microstructural evolution of NARloy-Z at elevated temperatures

Microstructural evolution was studied in samples of wrought and vacuum plasma sprayed (VPS) NARloy-Z exposed to temperatures up to 970 C (1,780 F) for up to 60 h. Samples were heated in a vacuum furnace, followed by rapid quenching in helium (He) gas at a cooling rate of 166 C (300 F) per second. Microstructural analyses were conducted using optical microscopy, scanning electron microscopy (SEM), and electron probe microanalysis (EPMA). In both the wrought and VPS conditions, precipitates rich in silver (Ag) and zirconium (Zr) were present in the matrix and at the grain boundaries even after long exposure to elevated temperatures. Islands rich in oxygen (O2) and Zr were also observed, as well as incipient melting at the grain boundary triple points. Results indicated that the alloy cannot be homogenized by heat treatment at elevated temperatures.

Singh, J.

Aubrite basalt vitrophyres: High sulfur silicate melts and a snapshot of aubrite formation

Two aubrite basalt vitrophyre clasts have been found within AMNH thin sections from the Parsa EH3 chondrite and the Khor Temiki aubrite. Polished sections of the Parsa Aubrite Inclusion (PAI) and the Khor Temiki Inclusion (KTI) were studied by optical, electron probe microanalysis (EPMA), and scanning electron microscopy (SEM) techniques with broad-beam and low absorbed EPMA currents used to minimize glass volatile loss. Some data have previously been reported for PAI and KTI may possibly correlate to a previously reported inclusion in Khor Tiimiki. In polished sections, PAI and KTI are approximately equal 4 mm in diameter and contain a large volume of glass. The clasts have similar textural characteristics and are akin to lunar vitrophyre textures. The glasses have high alkali rhyodacitic compositions Al-though PAI is peraluminous, KTI is significantly peralkaline. Additionally, the glasses have elevated sulfur concentrations that are extremely high by geochemical standards. SEM examination for beam overlap of microscopic CaS, FeS, and (Mg, Mn, Fe) S inclusions showed no such contamination. Furthermore, homogeneity of glass S content and low FeO contents help rule out contamination. Materials research data show that under reducing conditions alumino-silicate melts can dissolve up to several weight percent sulfur in the absence of Fe. The high S and alkali contents, the lack of associated high shock features, and the rationalized phase equilibria suggest that PAI and KTI are igneous melting products of an E-chondrite-like source material. Although large-scale impact melting cannot totally be ruled out, the above observations eliminate the possibility of in-situ shock melting.

Fogel, R. A.