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2012 | Buch

Introduction and Basic Concepts Kapitel lesen Erstes Kapitel lesen

Laser Techniques for the Study of Electrode Processes

verfasst von: Gyözö G. Láng, Cesar A. Barbero

Verlag: Springer Berlin Heidelberg

Buchreihe : Monographs in Electrochemistry

Enthalten in: Springer Professional "Wirtschaft+Technik" , Springer Professional "Technik"

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SUCHEN

Über dieses Buch

Laser-enabled measurements are valuable tools for the investigation of surfaces and interfaces or for the in situ investigation of interfacial processes including electrode processes. The understanding of the thermodynamics of solid/liquid surfaces is important for surface science and electrochemistry. In the first part of this book, the authors describe a range of techniques for investigating interfacial tension and surface stress, which is important for coatings, thin films, and fuel cells. The techniques covered comprise bending beam (bending plate, bending cantilever, wafer curvature) methods with different detection techniques. Special attention is given to methods using optical detection by laser beam deflection or interferometry. The second part is devoted to the techniques based on the detection of refractive index gradients in the solution. The refractive index changes could be related to concentration gradients (Probe Beam Deflection, PBD) or light-induced thermal gradients (Photothermal Deflection Spectroscopy, PDS). The application of the techniques to surface-confined and solution electrochemical systems is described. Subsequently, a comparison with others techniques able to monitor ion fluxes is performed.

Inhaltsverzeichnis

Frontmatter

Experimental Determination of Interfacial Stress Changes in Electrochemical Systems

Frontmatter
Chapter 1. Introduction and Basic Concepts
Abstract
Chapter 1 deals with the definitions of some general and specific terms concerning the electrochemistry of solid–liquid interfaces. The definitions of the terms “electrode” and “solid electrode” as well as selected concepts in electrochemistry and surface science are discussed. It has been stressed that a “solid electrode” is a multicomponent, multiphase electrochemical system, containing at least one solid phase, which means that it cannot be treated as a pure solid in vacuum. It has been concluded that in case of a “solid electrode,” the experimentally determinable quantity is the change of the intensive parameter conjugate to the interface area. This quantity is intimately related to the properties of the solid-liquid interface and not just to the properties of the surface of the solid phase; therefore, it seems reasonable to refer to it as the “interface stress change” or “interfacial stress change.”
Gyözö G. Láng, Cesar A. Barbero
Chapter 2. Elements of the Thermodynamic Theory of Electrified Interfaces
Abstract
In Chap. 2, several aspects of the thermodynamic theory and their physical interpretation are discussed, and a simple and concise treatment of electrified interfaces within the framework of classical thermodynamics is presented. Basic concepts such as “surface,” “interface,” “interphase,” “interfacial or interface region,” “dividing surface,” and “adsorption” are reviewed; Gibbs and Guggenheim models in interfacial thermodynamics are discussed. The derivation of the electrocapillary equation, the Lippmann equation, and the Gibbs adsorption equation for an ideally polarizable electrode is presented. An example for the application of the electrocapillary equation is provided. An equation has been derived for ideally polarizable electrodes for the case in which there is no complete equilibrium between the bulk of a solid and the interface.
Gyözö G. Láng, Cesar A. Barbero
Chapter 3. Some Problems Related to the Surface Thermodynamics of “Solid Electrodes”
Abstract
In this chapter, existing thermodynamic theories for solid–liquid interfaces are critically reviewed. The definition of the “generalized surface intensive parameter” is discussed. Some critical remarks have been made concerning the approach generally used in the literature. A brief review of the derivation of the “generalized Lippmann equation” held to be valid generally for solid electrodes is given. Special attention has been paid to the mathematical consequences of the homogeneous property of the fundamental equation. Inconsistencies in the derivation are cited. Problems related to the so-called “surface Gibbs−Duhem equation” are discussed. Some remarks concerning a recent theoretical debate on the derivation of the Shuttleworth equation are also included.
Gyözö G. Láng, Cesar A. Barbero
Chapter 4. Experimental Methods for the Measurement of Surface Stress Changes
Abstract
In Chap. 4, methods for the experimental determination of (interfacial) stress changes in electrochemical systems are presented. The piezoelectric method, the extensometer method and its variants (e.g., optical fiber interferometry with Mach–Zehnder interferometer), the “bending beam” (“bending cantilever,” “laser beam deflection,” “wafer curvature”) method and related techniques, and the method based on the measurement of contact angle are discussed in detail. Special attention has been paid to problems related to the use of the electrochemical bending beam and bending plate/disc methods. The theories of the methods are summarized, and typical experimental arrangements are presented. The kind and quality of information that can be achieved using these methods are discussed.
Gyözö G. Láng, Cesar A. Barbero
Chapter 5. Optical Detection of the Deformation
Abstract
In this chapter, optical methods for the experimental determination of interfacial stress changes in electrochemical systems are discussed. Typical experimental arrangements are presented (for “single beam” and the “multibeam” systems). The essential components of two frequently used methods—the “bending beam method” and “Kösters interferometry”—are lasers. The main difference between the two above techniques is the detection system: position sensing with photodiodes (“position-sensitive detectors,” PSD) in case of the bending beam method and automated detection of light intensity changes in case of the laser interferometer. Basic principles of these methods have been discussed. Possible sources of errors have been analyzed (effect of refraction, error due to nonnormal incidence or due to the lateral shift of the reflected laser beam at the optical window, errors related to the structure of the cantilever probe, etc.).
Gyözö G. Láng, Cesar A. Barbero
Chapter 6. Detection of the Cantilever Deflection by Microscopy
Abstract
In Chap. 6, advantages and limitations of some nonoptical techniques (e.g., scanning tunneling microscopy) used for the experimental determination of changes in cantilever deflection or for the measurement of the deformation of thin plates/disks in electrochemical systems are discussed. Typical experimental arrangements have been presented. Possible sources of errors (interaction forces between surfaces, clamping of probes, contact angles, design of the electrochemical cells) have been analyzed.
Gyözö G. Láng, Cesar A. Barbero
Chapter 7. Applications: Selected Experimental Results
Abstract
In this chapter, selected results of bending beam (bending plate) experiments with optical detection are presented as illustrative examples. In order to demonstrate the capabilities and limitations of stress measurements in electrochemical systems, relevant results obtained using the bending beam method and Kösters laser interferometry are discussed (e.g., platinum and gold in contact with electrolyte solutions, cyclic voltammetry and potential pulse experiments, stress changes in thin films and passive layers on metals, insertion of species into materials, monitoring of the electrochemical degradation of polymer films, simultaneous oscillations of electrode potential, surface mass and interfacial stress in the course of galvanostatic oxidation of formic acid on platinum, etc.).
Gyözö G. Láng, Cesar A. Barbero
Chapter 8. Mathematical Methods in Interfacial Thermodynamics
Abstract
This chapter gives a brief overview of the mathematical background, some important mathematical concepts, and various functional relationships underlying the thermodynamic theory of interfaces (theory of homogeneous functions and partly homogeneous functions, Euler’s theorem and the Gibbs–Duhem equation, and Legendre transformation). The extensive or intensive nature of thermodynamic variables is emphasized, and the relationship to the theory of homogeneous functions is presented. The mathematical principles are explained and illustrated with simple examples.
Gyözö G. Láng, Cesar A. Barbero

Probe Beam Deflection (PBD)

Frontmatter
Chapter 9. Introduction to Probe Beam Deflection Techniques
Abstract
The importance of probe beam deflection (PBD) techniques in the electrochemical field of study is evaluated. A review of the historical development of PBD techniques, and of the closely related photothermal deflection spectroscopy, is then performed.
Gyözö G. Láng, Cesar A. Barbero
Chapter 10. Basic Principles of Probe Beam Deflection Techniques
Abstract
The theoretical framework of probe beam deflection (PBD) techniques is described. First, the optical principles underlying the measurement are discussed. Then, the analytical solutions are presented for electrochemical systems subjected to different potentials and current perturbations. Among them are potential pulses (chronodeflectometry), current pulse, and sinusoidal perturbations. The behavior of continuous and discontinuous processes is discussed. The possibility to study multiflux processes by chronodeflectometry is explored. New techniques, such as normal pulse voltadeflectometry (NPVD) and differential pulse voltadeflectometry (DPVD), are proposed. Then, different approaches used to simulate or process the probe beam deflection data measured along cyclic voltammograms are discussed. Those include digital simulation, Laplace transform, and convolution. Finally, a typical experimental setup for PBD is described.
Gyözö G. Láng, Cesar A. Barbero
Chapter 11. Application of Probe Beam Deflection Techniques to the Study of Surface-Confined Electrochemical Systems
Abstract
Several probe beam deflection (PBD) studies of the ion exchange, occurring during electrochemical processes of surface-confined redox species, are described. Among them are the formation and reduction of oxide surface layers on noble metal electrodes, the double layer charging and specific ion adsorption on carbon and metal surfaces, the redox reactions of carbon surface groups, the charge compensation processes in electroactive oxides, redox and conductive polymer films, the irreversible oxidation of adsorbed species (e.g., CO), and the charge compensation processes in redox self-assembled multilayers. The systems are usually explored qualitatively using cyclic voltadeflectometry and the quantitatively analyzed using chronodeflectometry and/or diffusion deconvolution. The combination of the PBD measurements with other techniques (e.g., electrochemical quartz crystal microbalance) has proved to be useful to a more detailed insight on the ion exchange mechanism. The review of the published data suggests that surface-confined electrochemical systems are ideally suited to probe beam deflection measurements.
Gyözö G. Láng, Cesar A. Barbero
Chapter 12. Application of Probe Beam Deflection to Solution Electrochemical Systems
Abstract
The use of probe beam deflection (PBD) techniques to study solution electrochemical systems is described. The difficulties inherent on the data interpretation of the experimental measurements are discussed.
Gyözö G. Láng, Cesar A. Barbero
Chapter 13. In Situ Electrochemical Photothermal Deflection Techniques
Abstract
The theory of photothermal deflection spectroscopy (PDS) applied in situ to electrochemical systems is outlined. The predicted response to different forms of light excitation is described. Then, the experimental parameters relevant to the measurement of photothermal deflection signal in an electrochemical environment are discussed, along with the description of an actual photothermal deflection setup. Finally, experimental results of in situ electrochemical PDS and single wavelength photothermal deflection measurements are described. The techniques are compared with conventional optical absorption techniques such as transmission and reflectance spectroscopy.
Gyözö G. Láng, Cesar A. Barbero
Chapter 14. Comparison of Probe Beam Deflection Techniques with Other Methods to Monitor Fluxes of Mobile Species
Abstract
Different experimental techniques, which have been used to monitor the ion transport in electrochemical systems, are briefly reviewed. Among them are electrochemical techniques (scanning electrochemical microscopy, ring-disk rotating electrode, ion sensors), spectroelectrochemical techniques (in situ UV–visible spectroscopy with indicator dyes, infrared, and Raman), and various others (radiotracer detection, surface plasmon resonance, interferometry, electrochemical quartz crystal microbalance, etc.). The strengths and weakness of each technique is analyzed. In those cases where the same or similar systems have been also studied using PBD, the results are compared.
Gyözö G. Láng, Cesar A. Barbero
Backmatter
Metadaten
Titel
Laser Techniques for the Study of Electrode Processes
verfasst von
Gyözö G. Láng
Cesar A. Barbero
Copyright-Jahr
2012
Verlag
Springer Berlin Heidelberg
Electronic ISBN
978-3-642-27651-4
Print ISBN
978-3-642-27650-7
DOI
https://doi.org/10.1007/978-3-642-27651-4

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