The formation of a self-assembled monolayer (SAM) of 4-aminothiophenol (4-ATP) on polycrystalline platinum electrodes has been characterized by surface analysis and electrochemistry techniques. The 4-ATP monolayer was characterized by cyclic voltammetry (CV), linear sweep voltammetry, Raman spectroscopy, reflection-absorption infrared (RAIR) spectroscopy, and X-ray photoelectron spectroscopy (XPS). CV was used to study the dependence of the adsorption time and 4-ATP solution concentration on the relative degree of coverage of 4-ATP monolayers on polycrystalline Pt electrodes. The adsorption time range probed was 24-72 h. The optimal concentration of 4-ATP needed to obtain the highest surface at the lowest adsorption time was 10 mM. RAIR and Raman spectroscopy for 4-ATP-modified platinum electrodes showed the characteristic adsorption bands for 4-ATP, such as nuNH, nuCH(arom), and nuCS(arom), indicating the adsorption on the platinum surface. The XPS spectra for the modified Pt surface presented the binding energy peaks of sulfur and nitrogen. High energy resolution XPS studies, RAIR, and Raman spectrum for platinum electrodes modified with 4-ATP indicate that the molecules are sulfur-bonded to the platinum surface. The formation of a S-Pt bond suggests that ATP adsorption leads to an amino-terminated electrode surface. The thickness of the monolayer was evaluated via angle-resolved XPS (AR-XPS) analyses, giving a value of 8 A. As evidence of the terminal amino group on the electrode surface, the chemical derivatization of the 4-ATP SAM was done with 16-Br hexadecanoic acid. This surface reaction was followed by RAIR spectroscopy.
In this work, the sol-gel technology is used to produce silica based xerogels and aerogels
suitable for insulation applications in Space. The properties of the obtained materials are tailored
varying the precursor – Methyltrimethoxysilane (MTMS) or Methyltriethoxysilane (MTES), and the
solvent – methanol or ethanol. A two-step acid-base catalyzed synthesis is used, being the obtained
gels dried at atmospheric pressure, in the case of xerogels, and in supercritical conditions, for
aerogels. Density and thermal conductivity must be made as low as possible for the sought
application and only highly porous materials can fulfill this requirement. The obtained xerogels and
aerogels, either with MTMS or MTES, show very promising properties for thermal insulation in
Space, when methanol is used as solvent. The more suitable materials are obtained with MTMS and
exhibit very low density (80-100 kg/m3), very high surface area (~ 400 m2/g) and small pore size
(~ 30-40 Å). They also show moderate flexibility and a remarkable hydrophobic character (~ 150º).
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