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Synthesis and Structural Characterization of Tris(dimethyldithiocarbamate)Indium(III), In[S2CN(CH3)2]3

The synthesis and structure of the indium dithiocarbamate, In[SCN(CH3)2]3*1/2 4-mepy (4-mepy = 4-methylpyridine), is described. Indium metal was oxidized by tetramethylthiuramdisulfide in 4-methylpyridine at 25C to form a new, homoleptic indium(HI) dithiocarbamate in yields exceeding 60%. In[S2CN(CH3)213 exists as a discrete molecule with a distorted-octahedral geometry. The compound crystallizes in the P 1-bar (No. 2) space group with a = 9.282(l)A, b = 10.081(1)A, c = 12.502 A, alpha= 73.91 (1) degrees, beta = 70.21(1) degrees, gamma = 85.84(1) degrees, Z = 2,v(A(exp 3)) =1057.3(3), R = 0.046, and R(sub w) = 0.061.

Clark, Eric B.↗

Synthesis and Structural Characterization of Tris(dimethyldithicarbamate)Indium(III), In[S2CN(CH3)2]3

The synthesis and structure of the indium dithiocarbamate, In[S2CN(CH3)2]30 central dot 1/2 4- mepy (4-mepy = 4-methylpyridine), is described. Indium metal was oxidized by tetramethylthiuramdisulfide in 4-methylpyridine at 25 C to form a new, homoleptic indium(III) dithiocarbamate in yields exceeding 60%. In[S2CN(CH3)2]3 exists as a discrete molecule with a distorted-octahedral geometry. The compound crystallizes in the P 1-bar (No. 2) space group with a = 9.282(l) A, b = 10.081 (1) A, c, c = 12.502 A, alpha = 73.91 (1)(sup 0), beta = 70.21(1)(sup 0), gamma = 85.84(1)(sup 0), Z = 2, V (A(sup 3) = 1057.3(3), R = 0.046, and R(sub w) = 0.061.

Clark, Eric B.↗

Structural Characterization of Solar Silicon

Compared to single crystal silicon, solar silicon generally contains large residual stresses and numerous structural defects. During subsequent processing, the defect structure can undergo further changes since, at the high temperatures required for diffusion, dislocations are sufficiently mobile to rearrange themselves in patterns which reduce long range residual stresses. This process, which is similar to the polygonization of strained metals, has no counterpart in single crystal silicon. Many of the solar silicon materials are grown from graphite dies and crucibles and therefore contain carbon concentrations in excess of 1E18. The interactions between carbon, crystal defects, intrinsic point defects, oxygen and diffusing dopants are discussed.

Ast, D. G.↗

Electrical and Structural Characterization of Web Dendrite Crystals

Minority carrier lifetime distributions in silicon web dendrites are measured. Emphasis is placed on measuring areal homogeneity of lifetime, show its dependancy on structural defects, and its unique change during hot processing. The internal gettering action of defect layers present in web crystals and their relation to minority carrier lifetime distributions is discussed. Minority carrier lifetime maps of web dendrites obtained before and after high temperature heat treatment are compared to similar maps obtained from 100 mm diameter Czochralski silicon wafers. Such maps indicate similar or superior areal homogeneity of minority carrier lifetime in webs.

Schwuttke, G. H.↗

Electrical and Structural Characterization of Web Dendrite Crystals

Minority carrier lifetime distributions in silicon web dendrites are measured. Emphasis is placed on measuring areal homogeneity of lifetime, show its dependency on structural defects, and its unique change during hot processing. The internal gettering action of defect layers present in web crystals and their relation to minority carrier lifetime distributions is discussed. Minority carrier lifetime maps of web dendrites obtained before and after high temperature heat treatment are compared to similar maps obtained from 100 mm diameter Czochralski silicon wafers. Such maps indicate similar or superior areal homogeneity of minority carrier lifetime in webs.

Schwuttke, G. H.↗

Data structure characterization of miltispectral data using principal component and principal factor analysis

Both principal component analysis (PCA) and principal factor analysis (PFA) were used to analyze an experimental multispectral data structure in terms of common and unique variance. Only the common variance of the multispectral data was associated with the principal factor, while higher-order principal components were associated with both common and unique variance. The unique variance was found to represent small spectral variations within each cover type as well as noise vectors, and was most abundant in the lower-order principal components. The lower-order principal components can be useful in research designed to discriminate minor physical variations within features, and to highlight localized change when using multitemporal-multispectral data. Conversely, PFA of the multispectral data provided an insight into a great potential for discriminating basic land-cover types by excluding the unique variance which was related to the noise and minor spectral variations.

Lee, Jae K.↗

The Space Station structural characterization experiment

A space flight experiment being developed by NASA's Office of Aeronautics and Space Technology (OAST) that uses the Space Station as a testbed to study techniques for determining the dynamic characteristics of large space structures (LSS) is described. The experiment is separate from the Space Station Program itself with research objectives outside the domain of Space Station Program objectives. A brief description of the experiment, in terms of the general objective and approach, is given along with a statement of the potential benefits to NASA and others. The bulk of material to follow deals with the experiment definition activity that is underway. The scope of an 'initial' definition study and preliminary results from supporting Space Station dynamics analyses is presented. The term initial is used to indicate that the study currently being conducted has limited objectives and is not expected to complete the required experiment definition. A follow on study is planned and is mentioned in the summary.

Johnson, James W.↗

Structural Characterization of Crystalline Ice Nanoclusters

Water ice nanoclusters are useful analogs for studying a variety of processes that occur within icy grains in the extraterrestrial environment. The surface of ice nanoclusters prepared in the laboratory is similar to the surface of interstellar ice grains. In cold molecular clouds, the silicate cores of interstellar grains are typically approx. 100 nm in diameter and have a coating of impure amorphous water ice. Depositional, thermal and radiolytic processes leave the surface and subsurface molecules in a disordered state. In this state, structural defects become mobile and reactions of trapped gases and small molecules can occur. The large surface area of nanocluster deposits relative to their bulk allows for routine observation of such surface-mediated processes. Furthermore, the disordered surface and subsurface layers in nanocluster deposits mimic the structure of amorphous ice rinds found on interstellar dust grains. Transmission Electron Microscopy (TEM has been used tn characterize the crystallinity, growth mechanism, and size distribution of nanoclusters formed from a mixture of water vapor with an inert carrier gas that has been rapidly cooled to 77K. E M imaging reveals a Gaussian size distribution around a modal diameter that increases from approx. 15 to 30 nm as the percentage of water vapor within the mixture increases from 0.5 to 2.007, respectively . TEM bright and dark field imaging also reveals the crystalline nature of the clusters. h4any of the clusters show a mosaic structure in which crystalline domains originate at the center Other images show mirror planes that are separated by approx. 10 nm. Electron diffraction patterns of these clusters show that the clusters are composed of cubic ice with only a small hexagonal component. Further, the crystalline domain size is approximately the same as the modal diameter suggesting that the clusters are single crystals.

Blake, David↗

Processing-structure characterization of rheocast IN-100 superalloy

The rheocasting solidification process was applied in the production of IN-100 nickel base superalloy, and the effects of processing variables, such as stirring speed, isothermal stirring time, and volume fraction solid during isothermal stirring, on the resultant rheocast structure were investigated. Ingots that were furnace cooled at the same rate but without stirring were compared with the rheocast ingots. Rheocasting yielded fine-grained structures, where the extent of microsegregation, the variation in macrostructure, and the solidification-induced porosity and ingot cracking were found to be reduced in comparison to the unstirred ingots. The grain size and nonuniformity were reduced by increasing the stirring speed, isothermal stirring time, or the volume fraction solid during stirring; decreased microsegregation was achieved by an increase in the volume fraction solid. The structures of grain boundaries lent support to the grain boundary mechanism proposed by Vogel et al. (1977) for rheocasting.

Cheng, Jung-Jen Allen↗

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.↗

Forest Structure Characterization Using JPL's UAVSAR Multi-Baseline Polarimetric SAR Interferometry and Tomography

This paper concerns forest remote sensing using JPL's multi-baseline polarimetric interferometric UAVSAR data. It presents exemplary results and analyzes the possibilities and limitations of using SAR Tomography and Polarimetric SAR Interferometry (PolInSAR) techniques for the estimation of forest structure. Performance and error indicators for the applicability and reliability of the used multi-baseline (MB) multi-temporal (MT) PolInSAR random volume over ground (RVoG) model are discussed. Experimental results are presented based on JPL's L-band repeat-pass polarimetric interferometric UAVSAR data over temperate and tropical forest biomes in the Harvard Forest, Massachusetts, and in the La Amistad Park, Panama and Costa Rica. The results are partially compared with ground field measurements and with air-borne LVIS lidar data.

UAVSAR (Uninhabited Aerial Vehicle SAR)↗

Forest Structure Characterization Using Jpl's UAVSAR Multi-Baseline Polarimetric SAR Interferometry and Tomography

This paper concerns forest remote sensing using JPL's multi-baseline polarimetric interferometric UAVSAR data. It presents exemplary results and analyzes the possibilities and limitations of using SAR Tomography and Polarimetric SAR Interferometry (PolInSAR) techniques for the estimation of forest structure. Performance and error indicators for the applicability and reliability of the used multi-baseline (MB) multi-temporal (MT) PolInSAR random volume over ground (RVoG) model are discussed. Experimental results are presented based on JPL's L-band repeat-pass polarimetric interferometric UAVSAR data over temperate and tropical forest biomes in the Harvard Forest, Massachusetts, and in the La Amistad Park, Panama and Costa Rica. The results are partially compared with ground field measurements and with air-borne LVIS lidar data.

remote sensing↗

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi- component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma- sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia-yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging fiom 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗

Defect Clustering and Nano-Phase Structure Characterization of Multi-Component Rare Earth Oxide Doped Zirconia-Yttria Thermal Barrier Coatings

Advanced oxide thermal barrier coatings have been developed by incorporating multi-component rare earth oxide dopants into zirconia-yttria to effectively promote the creation of the thermodynamically stable, immobile oxide defect clusters and/or nano-scale phases within the coating systems. The presence of these nano-sized defect clusters has found to significantly reduce the coating intrinsic thermal conductivity, improve sintering resistance, and maintain long-term high temperature stability. In this paper, the defect clusters and nano-structured phases, which were created by the addition of multi-component rare earth dopants to the plasma-sprayed and electron-beam physical vapor deposited thermal barrier coatings, were characterized by high-resolution transmission electron microscopy (TEM). The defect cluster size, distribution, crystallographic and compositional information were investigated using high-resolution TEM lattice imaging, selected area diffraction (SAD), electron energy-loss spectroscopy (EELS) and energy dispersive spectroscopy (EDS) analysis techniques. The results showed that substantial defect clusters were formed in the advanced multi-component rare earth oxide doped zirconia- yttria systems. The size of the oxide defect clusters and the cluster dopant segregation was typically ranging from 5 to 50 nm. These multi-component dopant induced defect clusters are an important factor for the coating long-term high temperature stability and excellent performance.

Zhu, Dongming↗

High-Throughput Processes and Structural Characterization of Single-Nanotube Based Devices for 3D Electronics

We have developed manufacturable approaches to form single, vertically aligned carbon nanotubes, where the tubes are centered precisely, and placed within a few hundred nm of 1-1.5 micron deep trenches. These wafer-scale approaches were enabled by chemically amplified resists and inductively coupled Cryo-etchers to form the 3D nanoscale architectures. The tube growth was performed using dc plasmaenhanced chemical vapor deposition (PECVD), and the materials used for the pre-fabricated 3D architectures were chemically and structurally compatible with the high temperature (700 C) PECVD synthesis of our tubes, in an ammonia and acetylene ambient. The TEM analysis of our tubes revealed graphitic basal planes inclined to the central or fiber axis, with cone angles up to 30 deg. for the particular growth conditions used. In addition, bending tests performed using a custom nanoindentor, suggest that the tubes are well adhered to the Si substrate. Tube characteristics were also engineered to some extent, by adjusting growth parameters, such as Ni catalyst thickness, pressure and plasma power during growth.

top-down fabrication↗

Prochlorococcus phage ferredoxin: structural characterization and electron transfer to cyanobacterial sulfite reductases

Marine cyanobacteria are infected by phages whose genomes encode ferredoxin (Fd) electron carriers. These Fds are thought to redirect the energy harvested from light to phage-encoded oxidoreductases that enhance viral fitness, but it is unclear how the biophysical properties and partner specificities of phage Fds relate to those of photosynthetic organisms. Here, results of a bioinformatics analysis using a sequence similarity network revealed that phage Fds are most closely related to cyanobacterial Fds that transfer electrons from photosystems to oxidoreductases involved in nutrient assimilation. Structural analysis of myovirus P-SSM2 Fd (pssm2-Fd), which infects the cyanobacterium Prochlorococcus marinus, revealed high levels of similarity to cyanobacterial Fds (root mean square deviations of ≤0.5 Å). Additionally, pssm2-Fd exhibited a low midpoint reduction potential (–336 mV versus a standard hydrogen electrode), similar to other photosynthetic Fds, although it had lower thermostability (Tm = 28 °C) than did many other Fds. When expressed in an Escherichia coli strain deficient in sulfite assimilation, pssm2-Fd complemented bacterial growth when coexpressed with a P. marinus sulfite reductase, revealing that pssm2-Fd can transfer electrons to a host protein involved in nutrient assimilation. The high levels of structural similarity with cyanobacterial Fds and reactivity with a host sulfite reductase suggest that phage Fds evolved to transfer electrons to cyanobacterially encoded oxidoreductases.

cyanobacteria↗

Structural characterization and gas reactions of small metal particles by high-resolution TEM and TED

The interaction of 100 and 200 keV electron beams with amorphous alumina, titania, and aluminum nitride substrates and nanometer-size palladium particulate deposits was investigated for the two extreme cases of (1) large-area electron-beam flash-heating and (2) small-area high-intensity electron-beam irradiation. The former simulates a short-term heating effect with minimum electron irradiation exposure, the latter simulates high-dosage irradiation with minimum heating effect. All alumina and titania samples responded to the flash-heating treatment with significant recrystallization. However, the size, crystal structure, shape, and orientation of the grains depended on the type and thickness of the films and the thickness of the Pd deposit. High-dosage electron irradiation also readily crystallized the alumina substrate films but did not affect the titania films. The alumina recrystallization products were usually either all in the alpha phase, or they were a mixture of small grains in a number of low-temperature phases including gamma, delta, kappa, beta, theta-alumina. Palladium deposits reacted heavily with the alumina substrates during either treatment, but they were very little effected when supported on titania. Both treatments had the same, less prominent localized crystallization effect on aluminum nitride films.

Heinemann, K.↗

Frictional and structural characterization of ion-nitrided low and high chromium steels

Low Cr steels AISI 41410, AISI 4340, and high Cr austenitic stainless steels AISI 304, AISI 316 were ion nitrided in a dc glow discharge plasma consisting of a 75 percent H2 - 25 percent N2 mixture. Surface compound layer phases were identified, and compound layer microhardness and diffusion zone microhardness profiles were established. Distinct differences in surface compound layer hardness and diffusion zone profiles were determined between the low and high Cr alloy steels. The high Cr stainless steels after ion nitriding displayed a hard compound layer and an abrupt diffusion zone. The compound layers of the high Cr stainless steels had a columnar structure which accounts for brittleness when layers are exposed to contact stresses. The ion nitrided surfaces of high and low Cr steels displayed a low coefficient of friction with respect to the untreated surfaces when examined in a pin and disk tribotester.

Spalvins, T.↗