Synthesis of Silicalite-1 in Bicontinuous Microemulsion Containing AOT.

Silicalite-1 has been hydrothermally synthesized in a bicontinuous microemulsion of tetraethylenepentamine-sodium bis(2-ethylhexly) sulfosuccinate (AOT)-water system containing fluoride ions. The presence of AOT (an anionic surfactant) has been found to be essential for the formation of Silicalite-1 in bulk tetraethylene pentamine solvent. The tetrahedral binding sites of silicon atom have been confirmed by 29Si magic angle spinning NMR and FT-IR spectra. Thermogravimetric and differential thermal analysis studies on as-synthesized Silicalite-1 and X-ray diffraction pattern for calcined product established their structural stability. The scanning electron micrographs show the twinned and uniform morphology of crystals. The presence of additive (AOT) lengthens the nucleation period and helps to produce a large size crystal of Silicalite-1. Copyright 1999 Academic Press.

Effect of Co-Adsorbed Surfactant on the Structure of Self-Assembled Monolayer of Thiol on Polycrystalline Gold.

The structure and formation kinetics of a self-assembled monolayer (SAM) of long-chain alkane thiol in the presence and absence of an anionic surfactant like sodium dodecyl sulfate (SDS) has been studied using impedance, cyclic voltammetic, and quartz crystal microbalance (QCM) measurements. The comparison of these results, especially the ionic permeability of the monolayer, suggests a composite monolayer where both the surfactant and thiol molecules are cooperatively adsorbed to form distinct surfactant patches. This is further substantiated by the voltammetric experiments with redox probe in solution. A gradual change in the double layer capacitance value for the thiol monolayer alone (1.4 µF/cm2) to the composite monolayer (6.7 µF/cm2) and to the surfactant alone (11 µF/cm2) further supports the nature of the mixed monolayer. The kinetics of monolayer formation also shows interesting changes as revealed by the QCM studies, where a phase transition from simple to composite monolayer has been observed around an approximate coverage of 0.44. The same growth scheme is also observed for 1-pentanethiol, naphthalene disulfide, and diphenyl disulfide, suggesting that the mechanism appears to be general. Copyright 1998 Academic Press.