Differences in the location of guest molecules within zeolite pores as revealed by multilaser excitation confocal fluorescence microscopy: which molecule is where?

A detailed and systematic polarized confocal fluorescence microscopy investigation is presented on three batches of large coffin-shaped ZSM-5 crystals (i.e., parent, steamed at 500 °C, and steamed at 700 °C). In total, six laser lines of different wavelength in the visible region are employed on two crystal positions and three orientations with respect to the polarization plane of the excitation laser light. A fluorescent probe molecule is generated inside the zeolite pores, originating from the acid-catalyzed oligomerization of 4-fluorostyrene. A thorough analysis of the polarization plane of emitting fluorescent light reveals insight into the orientation of the fluorescent probe molecule restricted by the highly ordered zeolite channel framework, thereby visualizing pore accessibility and clearly distinguishing the occupation of straight and sinusoidal channels by the probe molecule. Spectral features are, furthermore, observed to tell apart molecules situated in one or the other pore. Special focus was given on the rim and tip regions of the zeolite ZSM-5 crystals. On the basis of the confocal approach of the investigation, the aforementioned features are evaluated in three dimensions, while the degradation of the zeolite framework upon postsynthesis steam treatment could be visualized by occupation of the sinusoidal pores

Heterogeneities of the Nanostructure of Platinum/Zeolite Y Catalysts Revealed by Electron Tomography

To develop structure-performance relationships for important catalysts, a detailed characterization of their morphology is essential. Using electron tomography, we determined in three dimensions the structure of Pt/zeolite Y bifunctional catalysts. Optimum experimental conditions enabled for the first time high-resolution 3D imaging of Pt particles as small as 1 nm located inside zeolite micropores. Semiautomated image analysis of 3D reconstructions provided an efficient study of numbers, size distributions, and interparticle distances of thousands of Pt particles within individual zeolite crystals. Upon extending this approach to a number of zeolite crystals of one batch of Pt/zeolite Y catalyst, heterogeneities were revealed. The Pt loading, an important parameter for catalyst performance, varied between zeolite crystals up to a factor of 35. This discovery calls for re-evaluation of catalyst preparation methods and suggests potential for lowering the nominal loading with noble metals