In situ Tomographic Imaging of a Silica-Supported Zirconocene-Based Catalyst Particle Using Holotomography

In olefin polymerization catalysts, fragmentation, i.e. the disintegration of the catalyst support due to polymer formation and build-up of mechanical stress at the active sites, is a process that decisively contributes to catalytic activity and, moreover, determines polymer characteristics. We propose to follow this process ‘live’ in individual catalyst particles under real operating conditions using high-resolution, full-field hard X-ray holotomography at beamline ID16B (ESRF). Due to its capacity to image at high speeds, the technique is suitable for imaging morphological changes to the particles in situ, thereby yielding unprecedented insights into polymer formation, crack propagation and active site generation. A newly developed MEMS ‘chip’-based microreactor system will be used to polymerize single silica-supported zirconocene-based catalyst particles under controlled conditions (p = 1–10 bar,RT) using a pulsing approach (alternating ethylene/inert gas feed)