Optical Investigation of the Intergrowth Structure and Accessibility of Brønsted Acid Sites in Etched SSZ-13 Zeolite Crystals by Confocal Fluorescence Microscopy

Abstract

Template decomposition followed by confocal fluorescence microscopy reveals a tetragonal-pyramidal intergrowth of subunits in micrometer-sized nearly cubic SSZ-13 zeolite crystals. In order to accentuate intergrowth boundaries and defect-rich areas within the individual large zeolite crystals, a treatment with an etching NaOH solution is applied. The defective areas are visualized by monitoring the spatial distribution of fluorescent tracer molecules within the individual SSZ-13 crystals by confocal fluorescence microscopy. These fluorescent tracer molecules are formed at the inner and outer crystal surfaces by utilizing the catalytic activity of the zeolite in the oligomerization reaction of styrene derivatives. This approach reveals various types of etching patterns that are an indication for the defectiveness of the studied crystals. We can show that specially one type of crystals, denoted as core-shell type, is highly accessible to the styrene molecules after etching. Despite the large crystal dimensions, the whole core-shell type SSZ-13 crystal is utilized for catalytic reaction. Furthermore, the confocal fluorescence microscopy measurements indicate a nonuniform distribution of the catalytically important Brønsted acid sites underlining the importance of space-resolved measurements.