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2021 | Buch

Electrochemical Methods of Nanostructure Preparation

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This book summarizes the electrochemical routes of nanostructure preparation in a systematic and didactic manner. It provides a comprehensive overview of electrodeposition, anodization, carbon nanotube preparation and other methods of nanostructure fabrication, combining essential information on the physical background of electrochemistry with materials science aspects of the field.

The book includes a brief introduction to general electrochemistry with an emphasis on physico-chemical aspects, followed by a description of the sample preparation methods. In each chapter, an overview of the particular method is accompanied by a discussion of the relevant physical or chemical properties of the materials, including magnetic, mechanical, optical, catalytic, sensoric and other features. While some preparation methods are discussed in connection with the theories of physical electrochemistry (e.g. electrodeposition), the book also covers methods that are more heuristic but nonetheless utilize electric current (e.g. anodization of porous alumina or synthesis of carbon nanotubes by means of electric arc discharge).

Inhaltsverzeichnis

Frontmatter

Background

Frontmatter
Chapter 1. Introduction
Abstract
This chapter shortly summarizes the history of chemical research related to size-dependent properties of materials from the early days of colloid chemistry to recent nanotechnologies. It is highlighted how electrochemical methods gained a role in processing of the nanosystems, making electrochemistry-based nanomanipulation methods an important part of the tool kit of today’s nanotechnology. The structure of the major part of the entire book and its topics are shortly presented.
László Péter
Chapter 2. Electrochemistry and Electrodeposition
Abstract
The present chapter offers a general overview on the basis of electrochemistry. This introduction deals also with concepts that are seldom discussed in electrochemistry monographs but that are necessary to bridge the gap between theoretical electrochemistry and plating practice. Basic crystallography is discussed in order to yield an atomic-level image on phase formation. Various empirical aspects of metal deposition are also outlined, including code position modes and structural aspects of coating formation.
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Chapter 3. Experimental Methods in Characterization of Nanosystems
Abstract
Although the present book is dedicated to the electrochemical preparation methods of nanostructures, it has to be recognized that even average-level publications use a handful of auxiliary methods for characterizing the samples synthesized essentially by any prepareation route. Therefore, a wide general knowledge of sample characterization methods is one of the essential qualifications of a successful materials scientist. While no in-depth insight can be offered in an introductory chapter for all possibly necessary characterization methods, this part yields a unique overview which may serve as the first step of the self-orientation of the reader.
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Nanostructured Materials Obtained by Using Non-structured Substrates of Large Surface Area

Frontmatter
Chapter 4. Ultrathin Layers
Abstract
This chapter presents electrodeposition methods in which the deposit thickness increment in a particular step of the process ranges up to a few monolayers. The discussion starts with the electrochemical analogy of layer-by-layer deposition methods, mostly based on alternating UPD of the components. This is followed with surface-limited redox replacement that also works on UPD principles. The next topic is the self-limiting deposition that is unrelated to UPD but also leading to layers of a few atomic layer thickness. Finally, atomic-scale imaging of the early phase of the metal deposition is summarized.
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Chapter 5. Compositionally Modulated and Multilayered Deposits
Abstract
The properites of compositionally modulated metals often differ significantly from their bulk counterparts. This makes the production of such layers an important tool, and the advantageous sample properties range from hardness through corrosion resistance to magnetization-related fields. This chapter summarizes the electrochemical methods of the deposition of compositionally (or layered) metals. Multiple-bath and single-bath methods are detailed, while the influence of the codeposition mode of the metals to be plated is also analyzed.  
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Chapter 6. Nanocrystalline Deposits
Abstract
Research on nanocrystalline materials has been in the forefront of materials science since the 1990s. Electrodeposition of nanocrystalline metals prooved to be a simple tool to produce a large variety of nanocrystalline metallic specimen with good reproducibility. After the summary of the major aspects of nanocrystallinity, peculiar features of several metallic elements and alloy groups are discussed. Special attention will be paid for electrochemical techniques used for the deposition of nanocrystalline metals.
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Chapter 7. Composites
Abstract
Composites prepared with electrodeposition techniques are unique because no analogous materials can be synthesized with alternative methods. The first part of this chapter deals with codeposited metals that yield composited either directly due the immiscibility of the components or upon annealing of the deposit. The second part of the chapter deals with deposits formed from pre-existing suspended particles in either cathodic or anodic processes. It is a special goal of the forthcoming treatment to distinguish cases when the composition of the particles incorporated into the deposit during the electrochemical process is of either no or high importance.
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Chapter 8. Porous Nanostructured Materials
Abstract
A large variety of electrochemical methods can be used to obtain porous nanostructures. The first part of this chapter deals with bottom-up methods such as dynamic bubble templating and direct deposition of porous layers, completed with post-deposition surface modification methods. The second part of the chapter yields an overview on dealloying, which is a top-down method to obtain porous nanostructures. In each part, combinative routes by applying various electrochemical and non-electrochemical methods are also be presented.
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Chapter 9. Electrosynthesis of Nanostructures Without a Coating Formation on Electrodes
Abstract
The common goal of electroplating is the production of a compact, well-adherent layer on the substrate. However, electrochemically assisted formation of nanoparticles in solutions is also possible. This chapter deals with methods in which at least one reactant of the solution reaction leading to the formation of particles is generated on an electrode. The reaction resulting in the particle formation may be electrochemical with charge transfer between the dissolved reactants or a simple precipitation.
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Nanostructured Materials Obtained by Using Structured Substrates and Other Special Electrode Arrangements

Frontmatter
Chapter 10. Electrochemical Manufacturing Methods Based on Surface Inhomogeneities at the Nanoscale
Abstract
Nanoscale inhomogeneities play an important role in the nucleation of a new phase on a substrate surface. Although such inhomogeneities occur in the surface of all polycrystalline metals, step edges on graphitic materials obtained an outstanding interest due to the negligible mobility of carbon atoms. First, nanostructured deposits will be dealt with where the step edges are of outstanding importance. Secondly, a few methods will be presented in which the surface inhomogeneities suitable for the nucleation of a new phase are produced intentionally, mostly with tip-based methods. After the discussion of such bottom-up methods, it will be presented how surface inhomogeneities of materials laminated naturally at the atomic scale can be exploited in top-down production of nanosheets and similar nanoobjects.
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Chapter 11. Templated Systems
Abstract
The present chapter deals with electrodeposition methods in which the shape of the deposit is determined by the geometrical constraints of a non-electroactive material exhibiting a condensed phase, which will be termed hereinafter as template. The condensed phase that constitutes the template is solid in most of the cases (nanoporous templates and those obtained by the self-assembly of sub-microscopic solid particles). In a few cases, the template-forming material is not solid; this is the case for either lyotropic templates that are liquid crystalline or molecular assemblies. The spatial constraint defined by the template has a much longer temporal stability than the typical deposition time of the nanoobjects into the template. Template preparation techniques are summarized shortly, and the emphasis is on the electrochemical methods used for creating nanostructures in the templates.
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Chapter 12. Localized or Spatially Selective Electrodeposition Methods
Abstract
This chapter summarizes methods of great variety in which the localization of the electrodeposition is a result of the presence of a thin reaction layer or the microscopic nature of at least one of the electrodes in the cell. Thin reaction layers can be found in classical thin-layer cells but also in electrochemical cells adapted for transmission electron microscopy. Although the geometry of the cell is not of the thin-layer configuration, polarizable liquid–liquid interfaces also provide a spatial constraint for the reaction zone. After the summary of the methods involving electrochemically active solid tips and nanopipettes, a few manufacturing procedures of micro- and nanoelectrodes are presented.
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High-Voltage Methods of Nanostructure Preparation

Frontmatter
Chapter 13. Preparation of Nanoporous Oxides from Metals by Electrochemical Anodization
Abstract
Anodization of metals with voltages above a few volts does not belong to the topic of classical electrochemistry, although it complies with all criteria of the electrochemical reactions. Namely, a chemical change is caused by the current that otherwise would not take place due to any collateral effect of the current passed. Therefore, anodization of metals is an important part of this summary, in particular taking into account its effect on the nanostructuring of the starting metal. The majority of the forthcoming discussion deals with aluminium and intends to give an overwise from traditional methods to new trends. Anodization of metals other than aluminium and that of alloys is also discussed shortly, highlighting the differences in the resulting nanostructured oxides.
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Chapter 14. Nanostructures Obtained with Plasma Discharge Processes
Abstract
Arc disharges provide en environment in which the reactions are related to the current passed and the formation of the products obtained cannot be achieved by merely the heat effect of the discharge. Therefore, reactions taking place in arc discharges can be classified as electrochemical reactions, even though they cannot be described with the same formalism as electrochemical reactions under ambient condtions. The products discussed in this chapter are primarily various carbon nanostructures, and a short outlook is given for metallic and ceramic nanoparticles synthesized by arc discharges.
László Péter
Backmatter
Metadaten
Titel
Electrochemical Methods of Nanostructure Preparation
verfasst von
Ph.D. László Péter
Copyright-Jahr
2021
Electronic ISBN
978-3-030-69117-2
Print ISBN
978-3-030-69116-5
DOI
https://doi.org/10.1007/978-3-030-69117-2

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