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.
Resorcinol-formaldehyde gels were produced at 50, 70 and 90°C and with three different R/C ratios (500, 1000 and 2000). The effect of these variables combined with that of aging time was studied in order to optimize the synthesis conditions. The convective air-drying process was used, and the drying duration was studied with regard to the synthesis conditions. The aging time has no effect on the pore texture after 24 h at 90°C or 48 h at 70°C, whatever the R/C value. The synthesis-aging step can be shortened by increasing the temperature.Nevertheless, the pore size tends then to decrease, especially when R/C is high, but this can be counterbalanced by increasing R/C. Moreover, bubbles often appear in the gel at high synthesis temperature, which limits the temperature to about 70°C in the case of monolithic parts. At 70°C and with an air velocity of 2 m/s, the elimination of 90% of the solvent Manuscript 2 requires 1 h drying when the pore size reaches 400-600 nm, 2.5 h for 50 nm wide pores and 3 h when the pore size decreases to 15-20 nm. The drying duration does not exceed 8 h in all cases and could be shortened by increasing the temperature at the end of the process.
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