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9783527313174

Diffraction and Spectroscopic Methods in Electrochemistry

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  • ISBN13:

    9783527313174

  • ISBN10:

    3527313176

  • Edition: 1st
  • Format: Hardcover
  • Copyright: 2006-09-11
  • Publisher: Wiley-VCH

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Summary

This ninth volume in the series concentrates on in situ spectroscopic methods and combines a balanced mixture of theory and applications, making it highly readable for chemists and physicists, as well as for materials scientists and engineers. As with the previous volumes, all the chapters continue the high standards of this series, containing numerous references to further reading and the original literature, for easy access to this new field. The editors have succeeded in selecting highly topical areas of research and in presenting authors who are leaders in their fields, covering such diverse topics as diffraction studies of the electrode-solution interface, thin organic films at electrode surfaces, linear and non-linear spectroscopy as well as sum frequency generation studies of the electrified solid-solution interface, plus quantitative SNIFTIRS and PM-IRRAS. Special attention is paid to recent advances and developments, which are critically and thoroughly discussed. The result is a compelling set of reviews, serving equally well as an excellent and up-to-date source of information for experienced researchers in the field, as well as as an introduction for newcomers.

Author Biography

Richard C. Alkire, Department of Chemical Engineering, University of Illinois, Urbana, USA

Dieter M. Kolb, Department of Electrochemistry, University of Ulm, Germany

Jacek Lipkowski, Department of Chemistry, University of Guelph, Canada

Philip N. Ross, Materials Science Department, Lawrence Berkeley National Laboratory, Berkeley, USA

Table of Contents

Series Preface V
Volume Preface XV
List of Contributors XVII
1 In-situ X-ray Diffraction Studies of the Electrode/Solution Interface
1(46)
Christopher A. Lucas and Nenad M. Markovic
1.1 Introduction
1(1)
1.2 Experimental
2(2)
1.3 Adsorbate-induced Restructuring of Metal Substrates
4(18)
1.3.1 Surface Relaxation
5(1)
1.3.1.1 Pt Monometallic and Bimetallic Surfaces
5(1)
1.3.1.2 Group IB Metals
12(4)
1.3.2 Surface Reconstruction
16(6)
1.4 Adlayer Structures
22(14)
1.4.1 Anion Structures
23(5)
1.4.2 CO Ordering on the Pt(111) Surface
28(3)
1.4.3 Underpotential Deposition (UPD)
31(5)
1.5 Reactive Metals and Oxides
36(5)
1.6 Conclusions and Future Directions
41(1)
Acknowledgments
42(1)
References
42(5)
2 UV-visible Reflectance Spectroscopy of Thin Organic Films at Electrode Surfaces
47(50)
Takamasa Sagara
2.1 Introduction
47(2)
2.2 The Basis of UV-visible Reflection Measurement at an Electrode Surface
49(1)
2.3 Absolute Reflection Spectrum versus Modulated Reflection Spectrum
50(3)
2.4 Wavelength-modulated UV-visible Reflectance Spectroscopy
53(1)
2.5 Potential-modulated UV-visible Reflectance Spectroscopy
54(1)
2.6 Instrumentation of the Potential-modulated UV-visible Reflection Measurement
55(2)
2.7 ER Measurements for Redox-active Thin Organic Films
57(5)
2.8 Interpretation of the Reflection Spectrum
62(3)
2.9 Reflection Measurement at Special Electrode Configurations
65(3)
2.10 Estimation of the Molecular Orientation on the Electrode Surface
68(5)
2.10.1 Estimation of the Molecular Orientation on the Electrode Surface using the Redox ER Signal
69(3)
2.10.2 Estimation of the Molecular Orientation on the Electrode Surface using the Stark Effect ER Signal
72(1)
2.11 Measurement of Electron Transfer Rate using ER Measurement
73(10)
2.11.1 Redox ER Signal in Frequency Domain
73(3)
2.11.2 Examples of Electron Transfer Rate Measurement using ER Signal
76(2)
2.11.3 Improvement in Data Analysis
78(1)
2.11.4 Combined Analysis of Impedance and Modulation Spectroscopic Signals
79(3)
2.11.5 Upper Limit of Measurable Rate Constant
82(1)
2.11.6 Rate Constant Measurement using an ER Voltammogram
82(1)
2.12 ER Signal Originated from Non-Faradaic Processes — a Quick Overview
83(1)
2.13 ER Signal with Harmonics Higher than the Fundamental Modulation Frequency
84(1)
2.14 Distinguishing between Two Simultaneously Occurring Electrode Processes
85(2)
2.15 Some Recent Examples of the Application of ER Measurement for a Functional Electrode
87(4)
2.16 Scope for Future Development of UV-visible Reflection Measurements
91(2)
2.16.1 New Techniques in UV-visible Reflection Measurements
91(1)
2.16.2 Remarks on the Scope for Future Development of UV-visible Reflection Measurements
92(1)
Acknowledgments
93(1)
References
93(4)
3 Epi-fluorescence Microscopy Studies of Potential Controlled Changes in Adsorbed Thin Organic Films at Electrode Surfaces
97(30)
Dan Bizzotto and Jeff L. Shepherd
3.1 Introduction
97(2)
3.2 Fluorescence Microscopy and Fluorescence Probes
99(1)
3.3 Fluorescence near Metal Surfaces
100(1)
3.4 Description of a Fluorescence Microscope for Electrochemical Studies
101(5)
3.4.1 Microscope Resolution
103(1)
3.4.2 Image Analysis
104(2)
3.5 Electrochemical Systems Studied with Fluorescence Microscopy
106(16)
3.5.1 Adsorption of C18OH on Au(111)
108(6)
3.5.2 The Adsorption and Dimerization of 2-(2'-Thienyl)pyridine (TP) on Au(111)
114(1)
3.5.3 Fluorescence Microscopy of the Adsorption of DOPC onto an Hg Drop
115(3)
3.5.4 Fluorescence Microscopy of Liposome Fusion onto a DOPC-coated Hg Interface
118(2)
3.5.5 Fluorescence Imaging of the Reductive Desorption of an Alkylthiol SAM on Au
120(2)
3.6 Conclusions and Future Considerations
122(1)
Structures and Abbreviations
123(1)
Acknowledgments
124(1)
References
124(3)
4 Linear and Non-linear Spectroscopy at the Electrified Liquid/Liquid Interface
127(36)
David J. Fermin
4.1 Introductory Remarks and Scope of the Chapter
127(1)
4.2 Linear Spectroscopy
128(18)
4.2.1 Total Internal Reflection Absorption/Fluorescence Spectroscopy
128(6)
4.2.2 Potential-modulated Reflectance/Fluorescence in TIR
134(5)
4.2.3 Quasi-elastic Laser Scattering (QELS)
139(3)
4.2.4 Other Linear Spectroscopic Studies at the Neat Liquid/Liquid Interface
142(4)
4.3 Non-linear Spectroscopy
146(8)
4.3.1 Second Harmonic Generation
146(5)
4.3.2 Vibrational Sum Frequency Generation
151(3)
4.4 Summary and Outlook
154(3)
Acknowledgments
157(1)
Symbols
157(1)
Abbreviations
158(1)
References
159(4)
5 Sum Frequency Generation Studies of the Electrified Solid/Liquid Interface
163(36)
Steven Baldelli and Andrew A. Gewirth
5.1 Introduction
163(11)
5.1.1 Theoretical Background
163(1)
5.1.2 SFG Intensities
164(1)
5.1.3 Resonant Term
165(1)
5.1.4 Non-resonant Term
166(1)
5.1.5 Phase Interference
167(1)
5.1.6 Orientation Information in SFG
168(1)
5.1.7 Phase Matching
169(1)
5.1.8 Surface Optics
169(2)
5.1.9 Data Analysis Reference
171(1)
5.1.10 Experimental Designs
172(1)
5.1.11 Spectroscopy Cell
173(1)
5.2 Applications of SFG to Electrochemistry
174(19)
5.2.1 CO Adsorption
176(1)
5.2.1.1 Polarization Studies
178(1)
5.2.1.2 Potential Dependence
178(1)
5.2.1.3 CO on Alloys
179(1)
5.2.1.4 Solvent Effects
180(1)
5.2.2 Adsorption of upd and opd H
180(1)
5.2.3 CN on Pt and Au Electrodes
180(1)
5.2.3.1 CN/Pt
180(1)
5.2.3.2 CN/Au
183(1)
5.2.4 OCN and SCN
183(1)
5.2.5 Pyridine and Related Derivatives
183(2)
5.2.6 Dynamics of CO and CN Vibrational Relaxation
185(2)
5.2.7 Solvent Structure
187(1)
5.2.7.1 Nonaqueous Solvents
187(1)
5.2.7.2 Aqueous Solvents
191(2)
5.2.8 Monolayers and Corrosion
193(1)
5.3 Conclusion
193(1)
Acknowledgments
194(1)
References
195(4)
6 IR Spectroscopy of the Semiconductor/Solution Interface
199(34)
Jean-Noël Chazalviel and François Ozanam
6.1 Introduction
199(1)
6.2 IR Spectroscopy at an Interface
200(3)
6.2.1 Basic Principles of IR Spectroscopy
200(1)
6.2.2 External versus Internal Reflection
201(2)
6.3 Practical Aspects at an Electrochemical Interface
203(4)
6.3.1 How Potential can Affect IR Absorption
204(1)
6.3.2 How to Isolate Potential-sensitive IR Absorption
205(2)
6.4 What can be Learnt from IR Spectroscopy at the Interface
207(10)
6.4.1 Vibrational Absorption of Interfacial and Double-Layer Species
208(3)
6.4.2 Vibrational Absorption of Species outside the Double-Layer
211(2)
6.4.3 Electronic Absorption
213(4)
6.5 Effect of Light Polarization in ATR Geometry
217(5)
6.5.1 Selection Rules for a Polarized IR Beam
218(1)
6.5.2 Case of Strongly Polar Species: LO-TO Splitting
218(4)
6.5.3 Polarization Modulation
222(1)
6.6 Dynamic Information from a Modulation Technique
222(2)
6.7 Case of Rough or Complex Interfaces
224(5)
6.7.1 Surface Roughness
225(1)
6.7.2 Composite Interface Films
226(3)
6.8 Conclusion
229(1)
References
230(3)
7 Recent Advances in in-situ Infrared Spectroscopy and Applications in Single-crystal Electrochemistry and Electrocatalysis
233(36)
Carol Korzeniewski
7.1 Introduction
233(1)
7.2 Experimental
234(4)
7.2.1 Spectrometer Systems
234(1)
7.2.2 Spectrometer Throughput Considerations
234(1)
7.2.3 Detectors
235(1)
7.2.4 Signal-to-Noise Ratio Considerations
236(1)
7.2.5 Signal Digitization
236(1)
7.2.6 Signal Modulation and Related Data Acquisition Methods
237(1)
7.3 Applications
238(24)
7.3.1 Adsorption and Reactivity at Well-defined Electrode Surfaces
238(1)
7.3.1.1 Adsorption on Pure Metals
238(1)
7.3.1.2 Electrochemistry at Well-defined Bimetallic Electrodes
241(3)
7.3.2 SEIRAS
244(5)
7.3.3 Infrared Spectroscopy as a Probe of Surface Electrochemistry at Metal Catalyst Particles
249(4)
7.3.4 Nanostructured Electrodes and Optical Considerations
253(1)
7.3.5 Emerging Instrumental Methods and Quantitative Approaches
254(1)
7.3.5.1 Step-scan Interferometry
254(1)
7.3.5.2 Two-dimensional Infrared Correlation Analysis
256(1)
7.3.5.3 Quantitation of Molecular Orientation
259(3)
7.4 Summary
262(1)
Acknowledgments
263(1)
References
263(6)
8 In-situ Surface-enhanced Infrared Spectroscopy of the Electrode/Solution Interface
269(46)
Masatoshi Osawa
8.1 Introduction
269(2)
8.2 Electromagnetic Mechanism of SE IRA
271(2)
8.3 Experimental Procedures
273(6)
8.3.1 Electrochemical Cell and Optics
273(3)
8.3.2 Preparation of Thin-film Electrodes
276(3)
8.4 General Features of SEIRAS
279(8)
8.4.1 Comparison of SEIRAS with IRAS
279(2)
8.4.2 Surface Selection Rule and Molecular Orientation
281(3)
8.4.3 Comparison of SEIRA and SERS
284(1)
8.4.4 Baseline Shift by Adsorption of Molecules and Ions
285(2)
8.5 Selected Examples
287(15)
8.5.1 Reactions of a Triruthenium Complex Self-assembled on Au
288(2)
8.5.2 Cytochrome c Electrochemistry on Self-assembled Monolayers
290(3)
8.5.3 Molecular Recognition at the Electrochemical Interface
293(3)
8.5.4 Hydrogen Adsorption and Evolution on Pt
296(2)
8.5.5 Oxidation of C1 Molecules on Pt
298(4)
8.6 Advanced Techniques for Studying Electrode Dynamics
302(7)
8.6.1 Rapid-scan Millisecond Time-resolved FT-IR Measurements
302(1)
8.6.2 Step-scan Microsecond Time-resolved FT-IR Measurements
303(5)
8.6.3 Potential-modulated FT-IR Spectroscopy
308(1)
8.7 Summary and Future Prospects
309(1)
Acknowledgments
310(1)
References
310(5)
9 Quantitative SNIFTIRS and PM IRRAS of Organic Molecules at Electrode Surfaces
315(62)
Vlad Zamlynny and Jacek Lipkowski
9.1 Introduction
315(1)
9.2 Reflection of Light from Stratified Media
316(9)
9.2.1 Reflection and Refraction of Electromagnetic Radiation at a Two-phase Boundary
317(6)
9.2.2 Reflection and Refraction of Electromagnetic Radiation at a Multiple-phase Boundary
323(2)
9.3 Optimization of Experimental Conditions
325(11)
9.3.1 Optimization of the Angle of Incidence and the Thin-cavity Thickness
327(3)
9.3.2 The Effect of Incident Beam Collimation
330(1)
9.3.3 The Choice of the Optical Window Geometry and Material
331(5)
9.4 Determination of the Angle of Incidence and the Thin-cavity Thickness
336(2)
9.5 Determination of the Isotropic Optical Constants in Aqueous Solutions
338(5)
9.6 Determination of the Orientation of Organic Molecules at the Electrode Surface
343(1)
9.7 Development of Quantitative SNIFTIRS
344(12)
9.7.1 Description of the Experimental Set-up
344(3)
9.7.2 Fundamentals of SNIFTIRS
347(1)
9.7.3 Calculation of the Tilt Angle from SNIFTIRS Spectra
348(1)
9.7.4 Applications of Quantitative SNIFTIRS
349(7)
9.8 Development of Quantitative in-situ PM IRRAS
356(17)
9.8.1 Introduction
356(1)
9.8.2 Fundamentals of PM IRRAS and Experimental Set-up
357(3)
9.8.3 Principles of Operation of a Photoelastic Modulator
360(4)
9.8.4 Correction of PM IRRAS Spectra for the PEM Response Functions
364(2)
9.8.5 Background Subtraction
366(2)
9.8.6 Applications of Quantitative PM IRRAS
368(5)
9.9 Summary and Future Directions
373(1)
Acknowledgments
373(1)
References
374(3)
10 Tip-enhanced Raman Spectroscopy-Recent Developments and Future Prospects 377(42)
Bruno Pettinger
10.1 General Introduction
377(2)
10.2 SERS at Well-defined Surfaces
379(5)
10.3 Single-molecule Raman Spectroscopy
384(7)
10.4 Tip-enhanced Raman Spectroscopy (TERS)
391(18)
10.4.1 Near-field Raman Spectroscopy with or without Apertures
391(4)
10.4.2 First TERS Experiments
395(6)
10.4.3 TERS on Single-crystalline Surfaces
401(8)
10.5 Outlook
409(1)
10.5.1 Recent Results
409(1)
10.5.2 New Approaches on the Horizon
409(1)
Acknowledgment
410(1)
References
411(8)
Subject Index 419

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