Vanadium Oxide: From Gels to Nanotubes

Vanadium oxide nanotubes (VO _x -NT) have been prepared by mixing hexadecylamine with V₂O₅·nH₂O gels. This procedure was followed by an hydrothermal treatment (150–180°C, 2–7 days) which leads to a large quantity of VO _x -NT. SEM and XRD analysis have been used to optimize the temperature and reaction time required for production of VO _x -Nt and morphology of the nanotubes investigated by TEM.     

Tetra-t-butyl magnesium phthalocyanine on gold: electronic structure and molecular orientation

In this work we have investigated the electronic structure and the molecular orientation of (t-Bu)(4)PcMg (tetra-t-butyl magnesium phthalocyanine) on polycrystalline and single crystalline gold substrates using photoemission spectroscopy and x-ray absorption spectroscopy, and we compare the results to the unsubstituted PcCu (copper phthalocyanine). The C 1s photoemission spectrum is described similar to unsubstituted relatives with an additional component for the aliphatic substituents. The variation of the excitation energy causes distinct differences in the shape of the C 1s spectrum, which is very useful for the analysis of the molecular orientation in the uppermost layer. It is shown that despite of the sterically demanding substituents, ordered sublimed films of (t-Bu)(4)PcMg are accessible, the orientation of the molecules, however, is different from the orientation of the unsubstituted relatives.     

Indium-mediated allylation/propargylation of α-diazoketones: a facile synthesis of 1-bromo-2-alkyl- or 2-arylpent-4-en-2-ols

α-Diazoketones undergo smooth allylation with successive bromide insertion with allylindium bromide generated in situ from allyl bromide and indium metal to produce 1-bromo-2-alkyl- or 2-arylpent-4-en-2-ols in high yields. Addition of propargylindium bromide produces 1-bromo-2-alkyl-or 2-arylpent-4-yn-2-ols under similar conditions.     

Studies on antimony oxides: Part I

Thermogravimetry (TG), differential thermal analysis (DTA) and X-ray diffraction studies of antimony(III) oxide, (Sb₂O₃), in air, nitrogen and argon atmospheres have been made. In air Sb₂O₃ becomes oxidized to Sb₂O₄ above 510°. The oxidation reaction proceeds in two stages as revealed by the TG and DTA curves. The behaviour of Sb₂O₃ is similar in both N₂ and Ar. Sb₂O₃ remains unaffected up to 430°, above which there is a slow, and continuous mass loss up to 550°. Above 550° Sb₂O₃ volatilizes resulting in an enormous weight loss. X-ray studies of the sublimate and the residue indicate the former to be the cubic form of Sb₂O₃ (Senarmontite) while the residue is the orthorhombic (Valentinite) structure. From the DTA curves in air, N₂ and Ar, the transition temperature for the cubic to the orthorhombic modification has been estimated to be around 610°.     

A carbazole-based polymeric azodye

A new polymeric azodye has been synthesized from carbazole by diazotization of its derivative N-methylcarbazole-3,6-diamine and subsequent coupling reaction with 2,2-bis(4-hydroxyphenyl-3-sulfonate-Na)-propane prepared from bisphenol-A. Its physico-chemical, electrical, and thermal properties have been characterized; finally, its application to the preparation of colored semiconductive films from polyvinyl alcohol has been studied.     

Polymerization of vinylcarbazole on copper(II)-13X molecular sieves: Role of copper(II) salts

Copper(II)-exchanged-13X molecular sieves, prepared from four copper(II) salts, namely, sulfate, nitrate, chloride, and acetate, and their activities in the polymerization of N-vinylcarbazole at a fixed copper ion exchange level were studied. From the kinetic characteristics of polymerization it was established that the variation in activities of the Cu-exchanged sieves is due primarily to the difference in the pH of the original salt solution, which is responsible for the varying degree of proton exchange with the zeolite during copper ion exchange. A first-order dependence of the rate of polymerization was observed with respect to H⁺ ion concentration of the original copper-salt solution. It was further established that the rate of polymerization of exchanged copper ion, at a hypothetical zero proton concentration, is low. A mechanism of polymerization of NVC on copper-exchanged-13X zeolite was suggested on the basis of the results obtained.