In–situ Characterization of Heterogeneous Catalysts

Helps researchers develop new catalysts for sustainable fuel and chemical production Reviewing the latest developments in the field, this book explores the in-situ characterization of heterogeneous catalysts, enabling readers to take full advantage of the sophisticated techniques used to study heterogeneous catalysts and reaction mechanisms. In using these techniques, readers can learn to improve the selectivity and the performance of catalysts and how to prepare catalysts as efficiently as possible, with minimum waste. In-situ Characterization of Heterogeneous Catalysts features contributions from leading experts in the field of catalysis. It begins with an introduction to the fundamentals and then covers: Characterization of electronic and structural properties of catalysts using X-ray absorption fine structure spectroscopy Techniques for structural characterization based on X-ray diffraction, neutron scattering, and pair distribution function analysis Microscopy and morphological studies Techniques for studying the interaction of adsorbates with catalyst surfaces, including infrared spectroscopy, Raman spectroscopy, EPR, and moderate pressure XPS Integration of techniques that provide information on the structural properties of catalysts with techniques that facilitate the study of surface reactions Throughout the book, detailed examples illustrate how techniques for studying catalysts and reaction mechanisms can be applied to solve a broad range of problems in heterogeneous catalysis. Detailed figures help readers better understand how and why the techniques discussed in the book work. At the end of each chapter, an extensive set of references leads to the primary literature in the field. By explaining step by step modern techniques for the in-situ characterization of heterogeneous catalysts, this book enables chemical scientists and engineers to better understand catalyst behavior and design new catalysts for green, sustainable fuel and chemical production.

CONTRIBUTORS vii Introduction: Goals and Challenges for the In–situ Characterization of Heterogeneous Catalysts 1 José A. Rodriguez, Jonathan C. Hanson, and Peter J. Chupas 1 QEXAFS in Catalysis Research: Principles, Data Analysis, and Applications 23 Anatoly I. Frenkel, Syed Khalid, Jonathan C. Hanson, and Maarten Nachtegaal 2 Spatially Resolved X–ray Absorption Spectroscopy 49 Christian G. Schroer and Jan–Dierk Grunwaldt 3 Energy–Dispersive EXAFS: Principles and Application in Heterogeneous Catalysis 75 Mark A. Newton and Andrew J. Dent 4 In–situ Powder X–ray Diffraction in Heterogeneous Catalysis 121 Jonathan Hanson and Poul Norby 5 Pair Distribution Function Analysis of High–Energy X–ray Scattering Data 147 Karena W. Chapman and Peter J. Chupas 6 Neutron Scattering for In–situ Characterization of Heterogeneous Catalysis 169 Ashfi a Huq and Wei–Ren Chen 7 Visualization of Surface Structures of Heterogeneous Catalysts under Reaction Conditions or during Catalysis with High–Pressure Scanning Tunneling Microscopy 191 Luan Nguyen, Shiran Zhang, Yingchun Ye, Yuan Zhu, Lei Wang, and Franklin (Feng) Tao 8 In–situ Infrared Spectroscopy on Model Catalysts 209 Kumudu Mudiyanselage and Darío J. Stacchiola 9 Infrared Spectroscopy on Powder Catalysts 241 Eli Stavitski 10 Structural Characterization of Catalysts by Operando Raman Spectroscopy 267 Gerhard Mestl and Miguel A. Bañares 11 In–situ Electron Paramagnetic Resonance of Powder Catalysts 293 Angelika Brückner 12 Application of Ambient–Pressure X–ray Photoelectron Spectroscopy for the In–situ Investigation of Heterogeneous Catalytic Reactions 315 David E. Starr, Hendrik Bluhm, Zhi Liu, Axel Knop–Gericke, and Michael Hävecker 13 Combined X–ray Diffraction and Absorption Spectroscopy in Catalysis Research: Techniques and Applications 345 Anatoly I. Frenkel and Jonathan C. Hanson 14 Combining Infrared Spectroscopy with X–ray Techniques for Interrogating Heterogeneous Catalysts 369 Mark A. Newton and Marcos Fernández–García 15 XRD–Raman and Modulation Excitation Spectroscopy 411 Wouter van Beek, Atsushi Urakawa, and Marco Milanesio 16 Catalyst Imaging Using Synchrotron–Based Multitechnique Approaches 441 Andrew M. Beale, Javier Ruiz–Martinez, and Bert M. Weckhuysen INDEX 475

JOSÉ A. RODRIGUEZ, PhD , is Senior Scientist at Brookhaven National Laboratory and Adjunct Professor in the Department of Chemistry of SUNY Stony Brook. Dr. Rodriguez's research efforts center on the application of new techniques for in-situ characterization to study catalysts used for the production of clean fuels. JONATHAN C. HANSON, PhD , is retired from the Department of Chemistry at Brookhaven National Laboratory. He continues to develop techniques to study catalytic processes under operando conditions at Brookhaven's National Synchrotron Light Source. PETER J. CHUPAS, PhD , is Group Leader of the Structural Science Group in the X-ray Science Division of the Advanced Photon Source at Argonne National Laboratory. Dr. Chupas develops new in-situ techniques and sample environments to characterize catalysts.