Vibrational Spectroscopy of Molecules on Surfaces

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1 Vibrational Spectroscopy of Molecules on Surfaces Edited by John T. Yates, Jr. University of Pittsburgh Pittsburgh, Pennsylvania and Theodore E. Madey National Bureau of Standards Gaithersburg, Maryland PLENUM PRESS NEW YORK AND LONDON

2 Contents 1. Normal Modes at Surfaces 1 N. V. Richardson and N. Sheppard 1. Introduction 1 2. The Vibrational Motions of Adsorbates at Surfaces 3 3. Spectroscopic Selection Rule Infrared and Raman Spectroscopy Vibrational Electron Energy Loss Spectroscopy (EELS) Other Vibrational Spectroscopies 8 4. Site Symmetries of the Adsorbent 9 5. The Vibrational Modes of Isolated Surface Adsorption Complexes Hydrogen on the (100) Face of a Cubic Metal Site Site Site CO Adsorbed Perpendicular to the (100) Face of a Cubic Metal N 2 Adsorbed Parallel to the Surface in the Bridge Site of a (100) Cubic Face Ethylene on Bridge Sites of (100) or (111) Metal Faces Two-Dimensional Adsorbate Arrays at Surfaces The Vibrations of Adsorbate Arrays c(2 x 2) Array of Adatoms in the Fourfold Hollow Site of the (100) Face of a Cubic Metal Bridge Site Adatom Occupancy of the (100) Surface of a Cubic Metal c(4 x 2) Structure for CO/Pt(lll) c(4 x 2) Structure for CO Adsorbed on Ni(lll) 36 * 7.5. (2 x 1) Structure for CO Adsorbed on Ni(U0) and Pd(110) Adsorbent Surface Modes c(2 x 2) Overlayers on Cu(100) (1 x 2) Reconstruction of Ir(110), Pt(110), and Au(110) 43 xi

3 xii Contents 9. Conclusion 45 References Excitation Mechanisms in Vibrational Spectroscopy of Molecules on Surfaces 49 J. W. Gadzuk 1. Introduction Why Vibrational Spectroscopy? Experimental Methods of Surface Vibrational Spectroscopy Infrared-Absorption Spectroscopy Surface-Enhanced Raman Spectroscopy Electron Energy Loss Spectroscopy Inelastic Tunneling Spectroscopy Neutron Inelastic Scattering Atomic Inelastic Scattering Theoretical Strategies Excitation Mechanisms Harmonic Oscillator Mechanics Free Oscillator Forced Oscillator Dynamic Dipoles Radiative Excitation Electronic Excitation Dipole Scattering Impact Scattering Resonance Excitation Neutron Excitation Line-shape Information Content Line-shape Generalities/Dephasing Localized Oscillator-Continuum Systems Electron-Hole Pairs Phonons Photons Summary and Generalizations Experimental Realization 96 References Infrared Spectroscopy of High-Area Catalytic Surfaces 105 A. T. Bell 1. Introduction Techniques for the Acquisition of Spectra Transmission Spectroscopy Diffuse-Reflectance Spectroscopy Photoacoustic Spectroscopy Sample Preparation 114

4 Contents xiii 4. Cell Designs Transmission Spectroscopy Diffuse-Reflectance and Photoacoustic Spectroscopies Ancillary Equipment Spectrometers Dispersive Spectrometers Fourier-Transform Spectrometers Comparison of Fourier-Transform and Dispersive Spectrometers Resolving Power Signal-to-Noise Ratio Data Acquisition, Storage, and Display Concluding Remarks 133 References Inelastic Electron Tunneling Spectroscopy 135 P. K. Hansma 1. Principles of the Method A Water Analogy Spectral Range, Sensitivity, Resolution, and Selection Rules Description of Typical Apparatus Apparatus for Sample Preparation Apparatus for Measuring Spectra Calibration, Artifacts, and Miscellaneous Problems Calibration Artifacts Junction Geometry Top Metal Electrode Cryogenic Temperatures Data Interpretation, Theory Peak Position Peak Widths Peak Intensities Examples of the Method's Use Overview of Applications The Study of Model Catalysts The Study of Corrosion Comparison with Other Techniques Conclusions 175 References Incoherent Inelastic Neutron Scattering: Vibrational Spectroscopy of Adsorbed Molecules on Surfaces 183 R. R. Cavanagh, J. J. Rush, and R. D. Kelley 1. Introduction Fundamental Physics of Neutron Scattering 185

5 xiv Contents 3. Experimental Modified Triple-Axis Spectrometer Time-of-Flight Spectrometry Sample Cells Sample Preparation Data Acquisition Analysis of Data Force Models and Vibrational Dynamics Neutron Spectra Diffusion and Reorientation Examples Hydrogen/Raney Nickel Hydrogen + Carbon Monoxide/Raney Nickel Hydrocarbons on Platinum Black Hydrocarbons in Zeolites Diffusive Motions Summary 217 References Electron Energy Loss Spectroscopy 223 N. R. Avery 1. Background The Spectrometer General Requirements The Energy Selectors The Electron Monochromator Input and Output Electron Optics Current Available from Electron Monochromator The Electron Source The Energy Analyzer The Suppressor Electron Detectors Construction Materials and Methods Materials Fabrication Methods Shielding Monochromator and Analyzer Power Supplies Operating an EEL Spectrometer Tuning Aligning the Beam Optimizing of the Beam Calibration Application of EELS to Surface Chemistry Experimental Surface Reaction Intermediate and Kinetics; Time-Resolved

6 Contents xv EELS 261 References Reflection Absorption Infrared Spectroscopy 267 В. Е. Hayden 1. Introduction Historical Development General Principles A Comparison with Other Techniques Experimental Considerations Optical Configuration Radiation Sources Monochromators and Interferometers Modulation Signal Detection Applications Selection Rules and the Adsorbate Geometry Vibrational Frequencies as Fingerprints Coverage-Dependent Frequency Shifts Dipole Coupling The Static Shift Natural Half-Widths and Line Shapes Intensities Outlook High-Resolution Vibrational Studies Catalysis on Single Crystals 339 References Raman Spectroscopy 345 A. Campion 1. Introduction Theory Classical: The Polarizability Tensor Quantum Mechanical: Selection Rules and Intensities Experimental Considerations Sensitivity and Surface Selectivity Single-Crystal Surfaces Electromagnetic Fields at Surfaces Angle-Resolved Measurements Selection Rules High Surface Area Materials Instrumentation Laser Sources Sample Configurations Single-Crystal Samples 380

7 xvi Contents High Surface Area Materials Conventional Detection Systems Scanning Monochromators Photomultipliers Counting electronics Multichannel detection Spectrographs Detector Arrays Examples and Applications Adsorbates on Single-Crystal Surfaces High Surface Area Materials Supports, Catalyst Structure Adsorbates Surface-Enhanced Raman Scattering Introduction Electromagnetic Enhancement Chemical Enhancement Applications of SERS Outlook 410 References Infrared Spectroscopy of Adsorbates on Metals: Direct Absorption and Emission 417 P. L. Richards and R. G. Tobin 1. Introduction Status of Relevant Technology Overview Photon Noise Detectors Spectrometers Conclusions for Surface Spectroscopy Direct Absorption Spectroscopy Techniques for Measurement of Absorbed Power Sensitivity of Thermal Detection The Direct Absorption Instrument Experimental Results: CO on Ag Surface Calorimetry Infrared Emission Spectroscopy The Emission Spectrometer Experimental Results: CO on Ni(100) Arrays and the Multichannel Advantage Nonequilibrium Emission and Chemiluminescence 458 References 459 Index 465

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