Mercury porosimetry applied to porous silica materials: successive buckling and intrusion mechanisms

in Colloids and Surfaces A : Physicochemical and Engineering Aspects (2001), 187

Some silica low-density xerogels exhibit two successive volume variation mechanisms, compaction and intrusion when submitted to mercury porosimetry. The position of the pressure of transition P-t between ... [more ▼]

Some silica low-density xerogels exhibit two successive volume variation mechanisms, compaction and intrusion when submitted to mercury porosimetry. The position of the pressure of transition P-t between the two mechanisms is characteristic of the tested material and allows to compute the buckling constant used to determine the pore size distribution in the compaction part of the experiment. The analysis of the mercury porosimetry data of a low-density xerogel wrapped in a tight membrane by the buckling law (intrusion is prevented and the sample is crushed during the whole porosimetry experiment) leads to a continuous unimodal distribution similar to the distribution of the unwrapped sample obtained by applying the buckling law below P-t and the intrusion law above P-t. This experiment confirms the validity of the use of the buckling law. The behaviour of the low-density xerogels can be related to one of their morphological characteristics. As the size of the aggregates of silica particles increases, the strength towards crushing increases and the change of mechanism from crushing to intrusion takes place at a lower pressure. (C) 2001 Elsevier Science B.V. All rights reserved. [less ▲]

The use of additives to prepare low-density xerogels

in Journal of Non-Crystalline Solids (2001), 285

Preparation of low-density xerogels by incorporation of additives during synthesis

in Journal of Non-Crystalline Solids (2001), 289(1-3), 88-96

Low-density xerogels were prepared by incorporation of an additive to alcogels prior to gelation. The additives studied are 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS), 3 ... [more ▼]

Low-density xerogels were prepared by incorporation of an additive to alcogels prior to gelation. The additives studied are 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS), 3-aminopropyltrimethoxysilane (AMS), propyltrimethoxysilane (PMS), tetramethylorthosilicate (TMOS) and 3-aminopropyltriethoxysilane (AES) using tetraethylorthosilicate (TEOS) as main silica precursor. Samples were also prepared with EDAS as additive and TMOS as main silica reagent. When the additive contains methoxy groups, it reacts first, forms nuclei on which the main reagent TEOS reacts to form the silica particles. The nucleation mechanism by the additive occurs only in case of a difference of reactivity between additive and main silica precursor. The other group of the additive (amine, alkyl group, ...) influences only the gelation time. In case of ethoxy groups (series AES/TEOS) or methoxy groups (series EDAS/TMOS) for both additive and main reagent, there is no nucleation by the additive. (C) 2001 Elsevier Science B.V. All rights reserved. [less ▲]

Characterization of porous polylactide foams by image analysis and impedance spectroscopy

in Langmuir (2000), 16(26), 10463-10470

The texture of highly porous polylactide foams prepared by freeze-drying of poly-L-lactide (L-PLA) and poly-DL-lactide (DL-PLA) solutions of various concentrations was investigated by two novel ... [more ▼]

The texture of highly porous polylactide foams prepared by freeze-drying of poly-L-lactide (L-PLA) and poly-DL-lactide (DL-PLA) solutions of various concentrations was investigated by two novel methodologies, image analysis and impedance spectroscopy. Image analysis of scanning electron micrographs of transverse cross-sections at two different magnifications gave information on both the macroporosity (1 mum < width 10 <mu>m) and ultramacroporosity (width > 10 mum). Impedance spectroscopy was used to investigate the transport properties of the three-dimensional porous matrices by measurement of ionic conduction. Image analysis showed that: (a) the macroporosity, which mainly contributes to porosity, is independent of the sample composition; (b) when the concentration of the polymer solution is increased, the density of the ultramacropores decreases and their average diameter increases; (c) the distribution of the ultramacropores is more homogeneous in the semicrystalline L-PLA. foams than in the amorphous DL-PLA counterparts, in which the ultramacropores tend to make clusters. The dielectric properties changed at low frequency, in relation to modifications in the ultramacroporosity. Ultramacropores of the L-PLA foams were found to be more open and more sensitive to the concentration of the polymer solutions compared with DL-PLA. Expectedly, the mechanical properties of the PLA foams changed with the structure of the ultramacroporous network. These results encourage further investigations on the texture of porous supports, to collect pertinent information on the physical macro- and ultramacroenvironment in which cells will reside. [less ▲]

Micropore size distributions of activated carbons

in Langmuir (2000), 16(16), 6754-6756

Characterization of porous polylactide foams by image analysis and impedance spectroscopy

in Langmuir (2000), 16(26), 10463-10470

Sequentially Compressive and Intrusive Mechanisms in Mercury Porosimetry of Carbon Blacks

in Journal of Colloid & Interface Science (1999), 217(1), 216-217

The mechanism of mercury penetration in two different commercial carbon blacks is studied. We show that the volume variation measured by mercury porosimetry in these systems is due to three successive ... [more ▼]

The mechanism of mercury penetration in two different commercial carbon blacks is studied. We show that the volume variation measured by mercury porosimetry in these systems is due to three successive mechanisms, which occur as the pressure increases: (1) mercury invasion of voids between macroscopic grains, (2) compaction and elastic compression of macroscopic grains, (3) intrusion in the voids of aggregates formed by primary particles. The cumulative surface calculated by the Rootare-Prenzlow equation (S(RP)) in the intrusion part and the BET surface area measured by nitrogen adsorption (S(BET)) are compared. Copyright 1999 Academic Press. [less ▲]

Preparation of low-density xerogels through additives to TEOS-based alcogels

in Journal of Non-Crystalline Solids (1999), 246(3), 216-228

A new process for preparing silica xerogels with similar textural properties to silica aerogels by drying under vacuum has been studied. The xerogels are produced by adding, before gelation, 3-(2 ... [more ▼]

A new process for preparing silica xerogels with similar textural properties to silica aerogels by drying under vacuum has been studied. The xerogels are produced by adding, before gelation, 3-(2-aminoethylamino)propyltrimethoxysilane (EDAS) to tetraethylorthosilicate (TEOS)-based alcogels, synthesised in a single base-catalysed (NH3) step. It is hypothesized that EDAS acts as a nucleation agent leading to silica particles with a hydrolysed EDAS core and a shell principally made of hydrolysed TEOS. The EDAS concentration and the basicity of the aqueous NH3 solution are important parameters influencing the resistance of the gel to drying stress. A decreasing EDAS/TEOS ratio or an increasing concentration of NH3 at constant EDAS content leads to less shrinkage during drying and so the final pore volume is larger. Gels prepared with a low EDAS/TEOS ratio (about 0.03) contain large particles (similar to 20 nm) due to the nucleation process by EDAS, thus the pores between those particles are also large and the drying stress is reduced. (C) 1999 Published by Elsevier Science B.V. All rights reserved. [less ▲]

Mercury porosimetry applied to low density xerogels; relation between structure and mechanical properties

in Journal of Sol-Gel Science and Technology (1998), 13(1-3), 335-339

Samples of low density xerogels were submitted to mercury porosimetry at pressures up to 200 MPa. These samples show an unusual behavior: they are first crushed by the isostatic mercury pressure without ... [more ▼]

Samples of low density xerogels were submitted to mercury porosimetry at pressures up to 200 MPa. These samples show an unusual behavior: they are first crushed by the isostatic mercury pressure without mercury intrusion and are then intruded by the mercury above a certain pressure. This transition allows the easy determination of the one constant found in the buckling model that is used to interpret the crushing part of the mercury porosimetry experiment. The relation between this constant and the structure of the xerogels determined by TEM and nitrogen adsorption is discussed. [less ▲]

Mercury porosimetry applied to low density xerogels

in Characterization of Porous Solids IV (1997)