Effects of carbon coating and pore corrugation on capillary condensation of nitrogen in SBA-15 mesoporous silica.

To examine the origin of an ink-bottle-like structure in SBA-15 formed by carbon coating and the effects of pore corrugation on capillary condensation and evaporation of a vapor in the cylindrical pores, we measured the adsorption isotherms of nitrogen at 77 K on 10 kinds of SBA-15 samples before and after a carbon coating process by the exposure to acetylene at 1073 K, as well as desorption scanning curves and subloops on the untreated samples. These SBA-15 samples were synthesized under the different conditions of initial SiO2/P123 ratio and hydrothermal treatment. SBA-15 with relatively large microporosity tends to form easily constrictions inside the main channels by the carbon coating. This strongly suggests that the rough pore walls of SBA-15 may induce the incomplete wetting of carbon layers on the pore walls to form the constrictions inside the cylindrical pores. A comparison of two subloops implies that the pores of SBA-15 synthesized with a SiO2/P123 ratio of 75 consist of an assembly of connecting domains of different diameters; that is, the pores are highly corrugated. For SBA-15 synthesized with a SiO2/P123 ratio of 60, the amplitude of the pore corrugation is significantly decreased by the prolonged hydrothermal treatment at 373 K. On the other hand, for SBA-15 synthesized with a SiO2/P123 ratio of 45, the amplitude of the corrugation is negligibly small, although the cylindrical pores are interconnected through narrow necks with each other. It is found that the smaller the amplitude of the pore corrugation, the smaller the width of the hysteresis loop.