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Isomerization of isocyanide into azulene by irradiation and formation from biphenylyl isothiocyanate, observing ring expansion and electrophilic carbenoid properties
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Azulene-doped naphtalene was directionally solidified using the vertical Bridgman-Stockbarger technique. Doping homogeneity and convection are determined as a function of the temperature profile in the furnace and the freezing rate. Convective velocities are two orders of magnitude lower when the temperature increases with height. The cross sectional variation in azulene concentration tends to be asymmetric. Neither rotation of the ampoule nor deliberate introduction of thermal asymmetries during solidification had a significant influence on cross sectional variations in doping. It is predicted that slow directional solidification under microgravity conditions can produce greater inhomogeneities than on earth. Thus when low freezing rates are necessary in order to avoid constitutional supercooling, it may be necessary to combine microgravity and magnetic fields in order to achieve homogeneous crystals.
Azulene-doped naphthalene was directionally solidified during the vertical Bridgman-Stockbarger technique. Doping homogeneity and convection were determined as a function of the temperature profile in the furnace and the freezing rate. Convection velocities were two orders of magnitude lower when the temperature increased with height. Rarely was the convection pattern axisymmetric, even though the temperature varied less than 0.1 K around the circumference of the growth ampoule. Correspondingly the cross sectional variation in azulene concentration tended to be asymmetric, especially when the temperature increased with height. This cross sectional variation changed dramatically along the ingot, reflecting changes in convection presumably due to the decreasing height of the melt. Although there was large scatter and irreproducibility in the cross sectional variation in doping, this variation tended to be least when the growth rate was low and the convection was vigorous. It is expected that compositional variations would also be small at high growth rates with weak convection and flat interfaces, although this was not investigated in the present experiments. Neither rotation of the ampoule nor deliberate introduction of thermal asymmetries during solidification had a significant influence on cross sectional variations in doping. It is predicted that slow directional solidification under microgravity conditions could produce greater inhomogeneities than on Earth. Combined use of microgravity and magnetic fields would be required to achieve homogeneity when it is necessary to freeze slowly in order to avoid constitutional supercooling.
The long range goal is to develop an improved understanding of phenomena of importance to directional solidification, to enable explanation and prediction of differences in behavior between solidification on Earth and in space. Emphasis during the period of this grant was on experimentally determining the influence of convection and freezing rate fluctuations on compositional homogeneity and crystalline perfection in the vertical Bridgman-Stockbarger technique. Heater temperature profiles, buoyancy-driven convection, and doping inhomogeneties were correlated using naphthalene doped with azulene. In addition the influence of spin-up/spin-down on compositional homogeneity and microstructure of indium gallium antimonide and the effect of imposed melting-freezing cycles on indium gallium antimonide are discussed.
Several celestial objects, including UV rich regions of planetary and reflection nebulae, stars, H II regions, and extragalactic sources, are characterized by the unidentified infrared emission bands (UIR bands). A few years ago, it was proposed that polycyclic aromatic hydrocarbon species (PAHs) are responsible for most of the UIR bands. This hypothesis is based on a spectrum analysis of the observed features. Comparisons of observed IR spectra with lab absorption spectra of PAHs support the PAH hypothesis. An example spectrum is represented, where the Orion Bar 3.3 micron spectrum is compared with the absorption frequencies of the PAHs Chrysene, Pyrene, and Coronene. The laser excited 3.3 micron emission spectrum is presented from a gas phase PAH (azulen). The infrared fluorescence theory (IRF) is briefly explained, followed by a description of the experimental apparatus, a report of the results, and discussion.