4.8 Article

FIB-SEM Tomography Probes the Mesoscale Pore Space of an Individual Catalytic Cracking Particle

Journal

ACS CATALYSIS
Volume 6, Issue 5, Pages 3158-3167

Publisher

AMER CHEMICAL SOC
DOI: 10.1021/acscatal.6b00302

Keywords

fluid catalytic cracking; focused ion beam-scanning electron microscopy; diffusion simulation; porous media; upscaling; transport ability

Funding

  1. NWO Gravitation program
  2. Netherlands Center for Multiscale Catalytic Energy Conversion (MCEC)
  3. European Research Council (ERC) [321140]

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The overall performance of a catalyst particle strongly depends on the ability of mass transport through its pore space. Characterizing the three-dimensional structure of the macro- and mesopore space of a catalyst particle and establishing a correlation with transport efficiency is an essential step toward designing highly effective catalyst particles. In this work, a generally applicable workflow is presented to characterize the transport efficiency of individual catalyst particles. The developed workflow involves a multiscale characterization approach making use of a focused ion beam-scanning electron microscope (FIB-SEM). SEM imaging is performed on cross sections of 10.000 mu m(2), visualizing a set of catalyst particles, while FIB-SEM tomography visualized the pore space of a large number of 8 mu m(3) cubes (subvolumes) of individual catalyst particles. Geometrical parameters (porosity, pore connectivity, and heterogeneity) of the material were used to generate large numbers of virtual 3D volumes resembling the sample's pore space characteristics, while being suitable for computationally demanding transport simulations. The transport ability, defined as the ratio of unhindered flow over hindered flow, is then determined via transport simulations through the virtual volumes. The simulation results are used as input for an upscaling routine based on an analogy with electrical networks, taking into account the spatial heterogeneity of the pore space over greater length scales. This novel approach is demonstrated for two distinct types of industrially manufactured fluid catalytic cracking (FCC) particles with zeolite Y as the active cracking component. Differences in physicochemical and catalytic properties were found to relate to differences in heterogeneities in the spatial porosity distribution. In addition to the characterization of existing FCC particles, our method of correlating pore space with transport efficiency does also allow for an up-front evaluation of the transport efficiency of new designs of FCC catalyst particles.

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