Application of Ambient Pressure X-ray Photoelectron Spectroscopy to Catalysis

APPLICATION OF AMBIENT PRESSURE X-RAY PHOTOELECTRON SPECTROSCOPY TO CATALYSIS Authoritative and detailed reference on ambient-pressure x-ray photoelectron spectroscopy for practitioners and researchers starting in the field Application of Ambient Pressure X-ray Photoelectron Spectroscopy to Catalysis introduces a relatively new analytical method and its applications to chemistry, energy, environmental, and materials sciences, particularly the field of heterogeneous catalysis, covering its background and historical development, its principles, the instrumentation required to use it, analysis of data collected with it, and the challenges it faces. The features of this method are described early in the text; the starting chapters provide a base for understanding how AP-XPS tracks crucial information in terms of the surface of a catalyst during catalysis. The second half of this book delves into the specific applications of AP-XPS to fundamental studies of different catalytic reactions. In later chapters, the focus is on how AP-XPS could provide key information toward understanding catalytic mechanisms. To aid in reader comprehension, the takeaways of each chapter are underlined. In Application of Ambient Pressure X-ray Photoelectron Spectroscopy to Catalysis, readers can expect to find detailed information on specific topics such as: Going from surface of model catalyst in UHV to surface of nanoparticle catalyst during catalysis Application of XPS from surface in UHV to surface in gas or liquid phase and fundamentals of X-ray spectroscopy Significance and challenges of studying surface of a catalyst in gaseous phase and instrumentation of ambient pressure X-ray photoelectron spectrometers Experimental methods of AP-XPS studies and difference in data analysis between AP-XPS and high vacuum XPS Ambient Pressure X-Ray Photoelectron Spectroscopy is an ideal resource for entry level researchers and students involved in x-ray photoelectron spectroscopy. Additionally, the text will appeal to scientists in more senior roles in academic and government laboratory institutions in the fields of chemistry, chemical engineering, energy science, and materials science. Cover Half Title Application of Ambient Pressure X-ray Photoelectron Spectroscopy to Catalysis Copyright Contents Preface 1. From Surface of Model Catalyst in UHV to Surface of Nanoparticle Catalyst During Catalysis References 2. Application of XPS: from Surface in UHV to Surface in Gas or Liquid Phase 2.1 Origin of X-ray Photoelectron Spectroscopy 2.2 Applications of XPS to Study Surface in High Vacuum 2.3 Applications of XPS to Study Sample in Gas Phase 2.4 Applications of XPS to Study Sample in Liquid Phase 2.4.1 XPS Studies of Surface of Nanoparticle Catalyst in Static Liquid 2.4.2 XPS Studies of Surface of Nanoparticle Catalyst in Flowing Liquid 2.4.3 XPS Study of Flowing Gas with a Pressure of 1 atm or Higher References 3. Fundamentals of X-ray Photoelectron Spectroscopy 3.1 Principle of XPS 3.2 Generation of X-ray 3.3 Excitation of Photoelectron and Chemical Shift 3.3.1 Initial State Effect 3.3.2 Final State Effect 3.3.2.1 Core Hole-Induced Polarization Final State Effect 3.3.2.2 Core Hole-Induced Rearrangement Final State Effect 3.4 Measurements of Energy of Photoelectrons 3.5 Measurements of Intensity of Photoelectrons References 4. Instrumentation of XPS 4.1 Regular X-ray Source 4.2 X-ray Source with a Monochromator 4.3 Energy Analyzer 4.4 Detector References 5. Significance and Challenge of Studying Surface of a Catalyst in Gaseous Phase 5.1 Origin of Difference between Surface in UHV and Surface in Reactant Gas 5.2 Intrinsic Feature of Catalytic Sites on Surface: Environmental Sensitivity 5.3 Ex Situ, Semi-in Situ, and In Situ/Operando Studies of Catalyst Surface at Ambient Pressure of Reactants 5.3.1 Difference among Ex Situ, Semi-In Situ, and In Situ/Operando Studies 5.3.2 Example of Surface Structures Only Formed and Maintained by Reactant at a Relatively High Pressure 5.3.3 Example of Catalyst Structure Only Observable during Catalysis 5.4 Ex Situ, Semi-in Situ, and In Situ/Operando Studies of Catalyst Structure at High Pressure 5.5 Technical Challenges in Studying Surface of a Catalyst in Gas Phase References 6. Instrumentation of Ambient Pressure X-ray Photoelectron Spectrometer 6.1 X-ray Source for AP-XPS Studies 6.1.1 Brief of X-ray Sources 6.1.2 Soft X-ray for AP-XPS and Its Limitation in High Pressure Studies 6.1.3 Al K for AP-XPS and Its Challenge in Working at Higher Pressure 6.1.4 Hard X-ray for AP-XPS and its Application to High Pressure Studies 6.2 Reaction Cell with Capability of Flowing Gas 6.2.1 Necessity of Having a Reaction Cell for Performing In Situ/Operando Studies of Catalysis 6.2.2 Structure of Reaction Cell 6.2.3 Sealing of a Reaction Cell and its Engaging Mechanism 6.2.4 Function of a Reaction Cell for AP-XPS Studies of Catalyst 6.3 Differential Pumping Energy Analyzer with High Transmission 6.4 Mass Spectrometer with Capability of Measurement of Catalytic Performance References 7. Experimental Methods of AP-XPS Studies 7.1 Leak Test of Reaction Cell 7.2 Exclusion of Catalysis by Reaction Cell 7.3 Tunning and Control of Sample-Aperture Distance 7.4 Sample Heating and Temperature Control 7.5 Online Measurement of Reactants and Products 7.6 Spectroscopic Titration of Surface Species References 8. Difference in Data Analysis Between AP-XPS and High Vacuum XPS 8.1 Potential Difference in Measuring Atomic Ratio of Two Elements on Catalyst Surface 8.2 Difference in Intensity of Photoelectrons Collected by Energy Analyzer 8.3 Difference in Resolution and Baseline of Spectrum 8.4 Difference in Spectrum between Free Molecules in Gas and Adsorbed Molecules on Surface 8.5 Calibration of Nominal Atomic Ratio A/Z of a Catalyst Surface in a Pure Gas 8.6 Calibration of Nominal Atomic Ratio A/Z of a Catalyst Surface in a Mixture of Reactants 8.7 Calibration of Nominal Atomic Ratio A/Z of a Catalyst Surface in a Pure Gas Obtained at Different Temperature for Fair Comparison References 9. Significance of Using AP-XPS in Studies of Catalysis 9.1 Fundamental of Catalyst Surface 9.2 Significance of Characterization of Surface of a Catalyst in Gas Phase 9.3 Significance of Using AP-XPS in Fundamental Studies of Catalysis References 10. CO Oxidation on Single Crystal Model Catalysts 10.1 Pt(557) and Pt(332) in CO 10.2 CO Oxidation on Pd(100), Pd(111), and Pd(110) 10.2.1 CO Oxidation on Pd(100) 10.2.2 CO Oxidation on Pd(111) 10.2.3 CO Oxidation on Pd(110) 10.3 CO Oxidation on Pt(110) and Pt(111) 10.3.1 CO Oxidation on Pt(110) 10.3.2 CO Oxidation on Pt(111) 10.4 CO Oxidation on Rh(110) 10.5 CO Oxidation on Cu(111) References 11. CO Oxidation on High Surface Area Catalysts 11.1 CO Oxidation on Rh Nanoparticles 11.2 CO Oxidation on Ru Nanoparticles References 12. Hydrogenation of Carbon Dioxide References 13. Water–Gas Shift 13.1 Co3O4 and Pt/Co3O4 13.1.1 Gas Composition-dependent Reducibility 13.1.2 Active Phase of Co3O4 during Water-Gas Shift 13.1.3 Active Phase of 0.5 wt% Pt/Co3O4 at 150–200 °C 13.1.4 Active Phase of 0.5 wt% Pt/Co3O4 at 280–350 °C 13.1.5 Temperature-dependent Evolution of Active Phase 13.2 Pt,Au, Pd, and Cu Supported on CeO2 Nanorods 13.3 CuO−Cr2O3−Fe2O3 References 14. Complete Oxidation of Methane 14.1 Complete Oxidation of Methane on NiCo2O4 14.2 Complete Oxidation of Methane on NiFe2O4 14.3 Complete Oxidation of Methane on NiO with Different Surface Structures References 15. Partial Oxidation of Methanol 15.1 Partial Oxidation of Methanol on Pd1Zn3/ZnO 15.2 Partial Oxidation of Methanol on Ir1Zn3/ZnO References 16. Partial Oxidation of Methane 16.1 Partial Oxidation of Methane on Pd/CeO2 16.2 Partial Oxidation of Methane on Pt/CeO2 16.3 Partial Oxidation of Methane on Rh/CeO2 References 17. Oxidative Coupling of Methane 17.1 OCM on Supported Na2WO4 and Hypothesized Active Phase Na2O2 17.2 First Observation of Na2O2 through AP-XPS Studies at 800 °C 17.3 Formation of a Thin Layer of Na2O2 Supported on Na2WO4 References 18. Dry and Steam Reforming of Methane 18.1 Dry Reforming of CH4 on CeO2 Anchored with Ni1 and Ru1 Sites 18.2 Steam Reforming of CH4 on CeO2 Anchored with Ni1 and Ru1 Single-atom Sites References 19. Reduction of NO with CO 19.1 Reduction of NO with CO on Co3O4 19.2 Reduction of NO with CO on Rh1Co3 Clusters Supported on CoO References 20. Tuning Catalyst Surfaces for Developing Catalysts 20.1 Capability of Compositional Restructuring Checkable with AP-XPS 20.2 Tracking Restructuring of Bimetallic Surface under Reaction and Catalytic Conditions for Tuning Catalytic Performance of a Bimetallic Catalyst References 21. Photocatalysis References Index