The observation of aerogels submitted to a pressure of mercury indicates that this porous material is compacted and not intruded by the mercury. Consequently, the classical Washburn equation cannot be applied. A relation is established between the pressure P of compaction and the size L of the largest pores. The size of pores is estimated by using the nitrogen adsorption-desorption isotherms analysis and SEM measurements. A relation is found in which P is proportional to L−4 The new relation is applied to mercury porosimetry. Finally, a mechanical model is proposed that reproduces successfully the behavior of aerogels under high pressure of mercury.
Time-resolved small-angle X-ray scattering (SAXS) measurements performed during the formation of tetraethyl
orthosilicate (TEOS) based silica gels in alcohol with 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS)
as an additive are reported. The measurements reveal no discontinuity of the nanostructure at the gel point.
A chemically induced spinodal phase separation is found to give a coherent picture of the collected data.
Increasing the amount of EDAS induces the phase separation on a smaller length scale, which finally leads
to a modified gel morphology. The SAXS measurements and the electron micrographs associated with the
dry gels could be interpreted in terms of the suggested wet gel formation mechanism.
Two carbon aerogels with different nanopore size distributions but both with high surface area, high nanoporous volume and low bulk density have been compared as platinum support. The influence of the nanostructure of the carbon aerogel on the platinum nanoparticle deposit was investigated. The platinum was deposited on the carbon by means of two different techniques, one employing an anionic platinum precursor, the other using a cationic one. The porosity of the carbon aerogels was characterized by combining N 2 -sorption and mercury porosimetry. The platinum deposit was characterized by transmission electron microscopy and rotating disk electrode experimentation to measure the platinum active surface area and its activity towards oxygen reduction reaction (ORR). The structural differences between the carbon aerogels did not yield any difference in platinum deposits in terms of Pt-surface area and ORR activity. Interestingly, the ORR mass activity of the high Pt-surface area samples, obtained by the cationic insertion technique, was several times lower than that of the samples obtained by the anionic technique. This observation was attributed to the particle size effect, detrimental in the case of platinum particle size around 1 nm.
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