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At least 19 records

Transmission Electron Microscopy (TEM) Sample Preparation of Si(1-x)Gex in c-Plane Sapphire Substrate

The National Aeronautics and Space Administration-invented X-ray diffraction (XRD) methods, including the total defect density measurement method and the spatial wafer mapping method, have confirmed super hetero epitaxy growth for rhombohedral single crystalline silicon germanium (Si1-xGex) on a c-plane sapphire substrate. However, the XRD method cannot observe the surface morphology or roughness because of the method s limited resolution. Therefore the authors used transmission electron microscopy (TEM) with samples prepared in two ways, the focused ion beam (FIB) method and the tripod method to study the structure between Si1-xGex and sapphire substrate and Si1?xGex itself. The sample preparation for TEM should be as fast as possible so that the sample should contain few or no artifacts induced by the preparation. The standard sample preparation method of mechanical polishing often requires a relatively long ion milling time (several hours), which increases the probability of inducing defects into the sample. The TEM sampling of the Si1-xGex on sapphire is also difficult because of the sapphire s high hardness and mechanical instability. The FIB method and the tripod method eliminate both problems when performing a cross-section TEM sampling of Si1-xGex on c-plane sapphire, which shows the surface morphology, the interface between film and substrate, and the crystal structure of the film. This paper explains the FIB sampling method and the tripod sampling method, and why sampling Si1-xGex, on a sapphire substrate with TEM, is necessary.

Kim, Hyun Jung↗

Structural characterization and gas reactions of small metal particles by high resolution in-situ TEM (Transmission Electron Microscopy) and TED (Transmission Electron Diffraction)

The detection and size analysis of small metal particles supported on amorphous substrates becomes increasingly difficult when the particle size approaches that of the phase contrast background structures of the support. An approach of digital image analysis, involving Fourier transformation of the original image, filtering, and image reconstruction was studied with respect to the likelihood of unambiguously detecting particles of less than 1 nm diameter on amorphous substrates from a single electron micrograph.

Heinemann, K.↗

Laboratory Investigation of the Growth and Crystal Structure of Nitric Acid Hydrates by Transmission Electron Microscopy (TEM)

A great deal of recent laboratory work has focussed on the characterization of the nitric acid hydrates, thought to be present in type I Polar Stratospheric Clouds (PSCs). Phase relationships and vapor pressure measurements (1-3) and infrared characterizations (4-5) have been made. However, the observed properties of crystalline solids (composition, melting point, vapor pressure, surface reactivity, thermodynamic stability, extent of solid solution with other components, etc.) are controlled by their crystal structure. The only means of unequivocal structural identification for crystalline solids is diffraction (using electrons, X-rays, neutrons, etc.). Other observed properties of crystalline solids, such as their infrared spectra, their vapor pressure as a function of temperature, etc. yield only indirect information about what phases are present, their relative proportions, or whether they are crystalline or amorphous.

Blake, David F.↗

Heterogeneous Distribution of Carbonaceous Material in Murchison Matrix: In Situ Observations Using Energy Filtered Transmission Electron Microscopy

Energy filtered TEM (Transmission Electron Microscopy) has been used to study the location of carbonaceous material in situ in Murchison matrix. Carbon occurs frequently as narrow rims around sulfide grains, but is rare in regions of matrix that are dominated by phyllosilicates. Additional information is contained in the original extended abstract.

Brearley, Adrian J.↗

The study of 'microsurfaces' using thermal desorption spectroscopy

The use of a newly combined ultrahigh vacuum technique for studying continuous and particulate evaporated thin films using thermal desorption spectroscopy (TDS), transmission electron microscopy (TEM), and transmission electron diffraction (TED) is discussed. It is shown that (1) CO thermal desorption energies of epitaxially deposited (111) Ni and (111) Pd surfaces agree perfectly with previously published data on bulk (111) single crystal, (2) contamination and surface structural differences can be detected using TDS as a surface probe and TEM as a complementary technique, and (3) CO desorption signals from deposited metal coverages of one-thousandth of a monolayer should be detectable. These results indicate that the chemisorption properties of supported 'microsurfaces' of metals can now be investigated with very high sensitivity. The combined use of TDS and TEM-TED experimental methods is a very powerful technique for fundamental studies in basic thin film physics and in catalysis.

Thomas, M. E.↗

Combustion of PTFE: The Effects of Gravity and Pigmentation on Ultrafine Particle Generation

Ultrafine particles generated during polymer thermodegradation are a major health hazard, owing to their unique pathway of processing in the lung. This hazard in manned spacecraft is poorly understood, because the particulate products of polymer thermodegradation are generated under low gravity conditions. Particulate generated from the degradation of PolyTetraFluoroEthylene (PTFE), insulation coating for 20 AWG copper wire (representative of spacecraft application) under intense ohmic heating were studied in terrestrial gravity and microgravity. Microgravity tests were done in a 1.2-second drop tower at the Colorado School of Mines (CSM). Thermophoretic sampling was used for particulate collection. Transmission Electron Microscopy (TEM) and Scanning Transmission Electron Microscopy (STEM) were used to examine the smoke particulates. Image software was used to calculate particle size distribution. In addition to gravity, the color of PTFE insulation has an overwhelming effect on size, shape and morphology of the particulate. Nanometer-sized primary particles were found in all cases, and aggregation and size distribution was dependent on both color and gravity; higher aggregation occurred in low gravity. Particulates from white, black, red and yellow colored PTFE insulations were studied. Elemental analysis of the particulates shows the presence of inorganic pigments.

McKinnon, J. Thomas↗

Effect of Pigmentation in Particulate Formation from Fluoropolymer Thermodegradation in Microgravity

Fires aboard spacecraft have occurred as a result of overheated electrical wires and thermodegradation of their insulation, which is composed of fluoropolymers. The particulate products of polymer thermodegradation are only 20-50 run in diameter and are thought to play a role in "polymer fume fever". Therefore an experimental study of the particulates produced by intense ohmic heating of various fluoropolymer-insulated 20 AWG copper wire (representative of spacecraft materials) was undertaken in normal gravity and in microgravity. The 2.2 s drop facility at NASA LeRC and 1.5 s drop facility at the Colorado School of Mines were used to achieve low gravity conditions. Thermophoretic sampling was used for particulate collection. Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM) were used to characterize the smoke particulates. It was found that the color of PTFE (Polytetrafluoroethylene) insulation has an overwhelming effect on the size, shape, morphology and, composition of the particulates. Size distributions and shape analyses using computerized image analysis showed that particle size distributions were also dependent on the pigment of the fluoropolymer insulation. The influence of pigment was observed in experiments under both normal and microgravity. Under microgravity conditions, owing to the lack of natural convective transport of particulates, much more particle aggregation was observed, and the nature of the aggregates was dependent on the color of the insulation.

Srivastava, Rajiv↗

Characterization and Analysis of Aerosol Particle Retention and Re-aerosolization from Hook-and-Loop Fasteners on the International Space Station

The extensive use of hook and loop fasteners aboard the International Space Station warrants careful examination of its contribution to indoor air pollution, as its fine fibers catch aerosol particles then re-aerosolize them upon being pulled apart, often within the breathing zone of astronauts. This problem is expanded by the lack of gravity because airborne particles larger than 1 micrometer do not settle. Instead these aerosols remain in the air until removed by filtration. Aerosol inhalation can have negative health effects, ranging from acute symptoms to long-term consequences, depending on particle sizes, mass and material composition. This study characterizes the size distribution, number concentration, and mass concentration of re-aerosolized debris generated by hook and loop fasteners taken from the stray light cover of the Microgravity Science Glovebox in the U.S. Laboratory of the ISS to understand the extent of its impact on air quality. Transmission electron microscopy (TEM) and scanning transmission electron microscopy (STEM), in conjunction with energy dispersive spectroscopy (EDS) were also used to characterize the morphology and composition of the particles.

Boyajian, Barbara↗

Correlated Microanalysis of Cometary Organic Grains Returned by Stardust

Preliminary examination (PE) of samples returned from Comet 81P/Wild 2 by the NASA Stardust mission revealed a wide variety of carbonaceous samples [e.g. 1]. Carbonaceous matter is present as inclusions, rinds, and films in polyminerallic terminal particles [2-4], as carbon-rich particles along track walls [2, 5, 6], and as organic matter in aerogel around tracks [7, 8]. The organic chemistry of these samples ranges from purely aliphatic hydrocarbons to highly-aromatic material, often modified by various organic functional groups [2, 4, 5, 9-11]. Difficulty arises when interpreting the genesis of these carbonaceous samples, since contaminants could be introduced from the spacecraft [12], aerogel [1, 8], or during sample preparation. In addition, hypervelocity capture into aerogel may have heated cometary material in excess of 1000 C, which could have significantly altered the structure and chemistry of carbonaceous matter. Fortunately, much of this contamination or alteration can be identified through correlated microanalysis with transmission electron microscopy (TEM), scanning-transmission X-ray microscopy (STXM), and nanoscale secondary ion mass spectroscopy (SIMS).

DeGregorio, B. T.↗

Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

Source record↗

TEM Study of Precipitation in a NiAl-3Ti-0.5Hf Single-Crystal Alloy

Samples for transmission electron microscopy (TEM) were prepared from 3 mm diameter cylinders electro-discharge machined from the heat-treated ingots. Slices sectioned from the cylinders were mechanically ground and electrochemically thinned in a twinjet Tenupol-3 polisher. Microstructural and energy-dispersive X-ray spectroscopy (EDXS) studies were conducted in a Philips 400T TEM equipped with a double tilt goniometer and a KEVEX Si/Li X-ray detector.

Garg, A.↗

Xenoliths in the CM2 Carbonaceous Chondrite LON 94101: Implications for Complex Mixing on the Asteroidal Parent Body

Xenoliths are foreign clasts that oc-cur in various classes of meteorites, e.g. [1,2,3]. A re-cent study reveals the presence of several distinct classes of xenoliths in regolith-bearing meteorites, in-cluding in over 20 different carbonaceous chondrites [4]. The most common types of xenoliths are fine-grained hydrous clasts, often referred to as C1 or CI clasts in the literature, although their mineralogy is actually more similar to hydrous micrometeorites [5,6]. Xenoliths in meteorites present an opportunity to study material not yet classified or available as separate meteorites, and can provide additional information on processes in the dynamic early history of the Solar Sys-tem. Here we have performed chemical and mineralogi-cal analyses of xenoliths in the CM2 carbonaceous chondrite LON 94101, using scanning electron micro-scopy (SEM) and transmission electron microscopy (TEM).

Lindgren, P.↗

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

SiC fiber-bonded ceramics (SA-Tyrannohex: SA-THX) diffusion-bonded with TiCu metallic interlayers were investigated. Thin samples of the ceramics were prepared with a focused ion beam (FIB) and the interfacial microstructure of the prepared samples was studied by transmission electron microscopy (TEM) and scanning TEM (STEM). In addition to conventional microstructure observation, for detailed analysis of reaction compounds in diffusion-bonded area, we performed STEM-EDS measurements and selected area electron diffraction (SAD) experiments. The TEM and STEM experiments revealed the diffusion-bonded area was composed of only one reaction layer, which was characterized by TiC precipitates in Cu-Si compound matrix. This reaction layer was in good contact with the SA-THX substrates, and it is concluded that the joint structure led to the excellent bonding strength.

Ceramics↗

A Survey of Jet Aircraft PM by TEM in APEX III

Based upon field testing during the NASA led APEX III campaign conducted in November 2005 at the NASA Glenn Research Center in coordination with Continental Airlines and Cleveland Hopkins International Airport. This paper reports observations of particulate emissions collected from a suite of jet engine aircraft to assess differences and similarities in soot macro- micro- and nanostructure using transmission electron microscopy (TEM). Aggregates are compact, primary particle sizes varied and nanostructure mixed. Comparisons are made to more familiar laboratory flame-generated soot as a well-studied point of reference. Results are interpreted in terms of turbulence interacting with the different stages of particle formation and growth.

soot↗

TEM Analysis of Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

Silicon Carbide (SiC) is a promising material for thermostructural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, Mo-B and TiCu. In this presentation, we report the microstructure of diffusion bonded SA-THX mainly with TiCu interlayers obtained by TEM observations, and the influence of metallic interlayers on the joint microstructure and microhardness will be discussed.

Ceramics↗

TEM Analysis of Interfaces in Diffusion-Bonded Silicon Carbide Ceramics Joined Using Metallic Interlayers

Silicon Carbide (SiC) is a promising material for thermo-structural applications due to its excellent high-temperature mechanical properties, oxidation resistance, and thermal stability. However, joining and integration technologies are indispensable for this material in order to fabricate large size and complex shape components with desired functionalities. Although diffusion bonding techniques using metallic interlayers have been commonly utilized to bond various SiC ceramics, detailed microstructural observation by Transmission Electron Microscopy (TEM) of the bonded area has not been carried out due to difficulty in preparing TEM samples. In this study, we tried to prepare TEM samples from joints of diffusion bonded SiC ceramics by Focused Ion Beam (FIB) system and carefully investigated the interfacial microstructure by TEM analysis. The samples used in this study were SiC fiber bonded ceramics (SA-Tyrannohex: SA-THX) diffusion bonded with metallic interlayers such as Ti, TiMo, and Mo-B. In this presentation, the result of microstructural analysis obtained by TEM observations and the influence of metallic interlayers and fiber orientation of SA-THX on the joint microstructure will be discussed.

Silicon Carbide↗