0000000000347219
AUTHOR
Zelimir Gabelica
Characterization of [Cu]-MCM-41 by XPS and CO or NO adsorption heat measurements
We report the characterization of copper doped MCM-41 prepared by original direct synthesis by XPS and adsorption calorimetry of CO and NO, which are selective molecular probes for Cu(I) and Cu(II) respectively. Investigation of the nature of the copper ions in this particular calcined Cu-MCM-41 by NO adsorption calorimetry shows that two types of energetically distinct adsorption sites exist, meaning the presence of two populations of Cu(II) species differently coordinated to the silica surface in quasi-equimolar concentration, as ascertained by XPS data. A small amount of Cu(I) was also detected, probably stemming from a partial reduction upon the successive vacuum treatments. The respect…
Pore shape affects the determination of the pore size of ordered mesoporous silicas by mercury intrusion.
MCM-41 and SBA-15 micelle-templated silicas are ideal reference materials to study the effect of surface roughness on pore size measurement by mercury intrusion, as the inner surface of the mesoporous channels is much rougher in the case of SBA-15 than MCM-41. In the case of MCM-41, the pressure of mercury intrusion is related to the pore size by the classical Washburn−Laplace law, while in the case of SBA-15, the pressure of intrusion is much higher than expected and classical models underevaluate the size of the channels. Defects on the pore surface of SBA-15 affect the mercury intrusion in a similar way as the deviation from cylindrical geometry does for the pores of spongelike silica gl…