xii
Contents
9.1.2
Mediated Formation of Metal Nanoparticles
with Electrochemical Generation of a Reducing
Agent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 306
9.2 Metal Oxide Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309
9.2.1
General Aspects of the Electrosynthesis of Free
Oxide Particles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309
9.2.2
Cathodic Processes for Obtaining Iron Oxide
Particles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310
9.2.3
Iron Oxide Synthesis with Sacrificial Anodes . . . . . . . . 313
9.2.4
Co-precipitation of Mixed Magnetic Oxide
Particles Containing Iron . . . . . . . . . . . . . . . . . . . . . . . . . 315
9.3 Electrochemically Assisted Synthesis of Miscellaneous
Non-metallic Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 316
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 317
Part III Nanostructured Materials Obtained by Using Structured
Substrates and Other Special Electrode Arrangements
10 Electrochemical Manufacturing Methods Based on Surface
Inhomogeneities at the Nanoscale . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 323
10.1 Pulse Sequences for the Regulation of Nucleation, Growth
and Post-deposition Treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 323
10.2 Electrodeposition of Nanocrystals . . . . . . . . . . . . . . . . . . . . . . . . . . 326
10.2.1 General Aspects of the Electrochemical
Nucleation of Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . 326
10.2.2 Substrate–Nanoparticles Pairs and Deposition
Conditions for Nanoparticle Preparation . . . . . . . . . . . . 327
10.3 Electrodeposition on Surfaces with Step Edges . . . . . . . . . . . . . . . 328
10.3.1 General Considerations Concerning
the Deposition Along Step Edges . . . . . . . . . . . . . . . . . . 328
10.3.2 Deposition on the Step Edges of Graphite . . . . . . . . . . . 330
10.4 Electrodeposition on Surfaces with Mechanically Induced
Nanoinhomogeneities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 337
10.5 Top-Down Electrochemical Synthesis of Nanosheets . . . . . . . . . . 341
10.5.1 Intercalation and Accompanying Exfoliation
Processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341
10.5.2 Graphene by Electrochemical Exfoliation
from Aqueous Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . 343
10.5.3 Graphene by Electrochemical Exfoliation
from Solutions with Non-aqueous Solvents . . . . . . . . . . 346
10.5.4 Electrochemistry-Based Transfer Methods
of Graphene and Graphene Oxide Nanosheets . . . . . . . 347
10.5.5 Electrochemical Exfoliation of Various Inorganic
Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 348
Contents
9.1.2
Mediated Formation of Metal Nanoparticles
with Electrochemical Generation of a Reducing
Agent . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 306
9.2 Metal Oxide Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309
9.2.1
General Aspects of the Electrosynthesis of Free
Oxide Particles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 309
9.2.2
Cathodic Processes for Obtaining Iron Oxide
Particles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 310
9.2.3
Iron Oxide Synthesis with Sacrificial Anodes . . . . . . . . 313
9.2.4
Co-precipitation of Mixed Magnetic Oxide
Particles Containing Iron . . . . . . . . . . . . . . . . . . . . . . . . . 315
9.3 Electrochemically Assisted Synthesis of Miscellaneous
Non-metallic Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 316
References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 317
Part III Nanostructured Materials Obtained by Using Structured
Substrates and Other Special Electrode Arrangements
10 Electrochemical Manufacturing Methods Based on Surface
Inhomogeneities at the Nanoscale . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 323
10.1 Pulse Sequences for the Regulation of Nucleation, Growth
and Post-deposition Treatment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 323
10.2 Electrodeposition of Nanocrystals . . . . . . . . . . . . . . . . . . . . . . . . . . 326
10.2.1 General Aspects of the Electrochemical
Nucleation of Nanoparticles . . . . . . . . . . . . . . . . . . . . . . . 326
10.2.2 Substrate–Nanoparticles Pairs and Deposition
Conditions for Nanoparticle Preparation . . . . . . . . . . . . 327
10.3 Electrodeposition on Surfaces with Step Edges . . . . . . . . . . . . . . . 328
10.3.1 General Considerations Concerning
the Deposition Along Step Edges . . . . . . . . . . . . . . . . . . 328
10.3.2 Deposition on the Step Edges of Graphite . . . . . . . . . . . 330
10.4 Electrodeposition on Surfaces with Mechanically Induced
Nanoinhomogeneities . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 337
10.5 Top-Down Electrochemical Synthesis of Nanosheets . . . . . . . . . . 341
10.5.1 Intercalation and Accompanying Exfoliation
Processes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 341
10.5.2 Graphene by Electrochemical Exfoliation
from Aqueous Solutions . . . . . . . . . . . . . . . . . . . . . . . . . . 343
10.5.3 Graphene by Electrochemical Exfoliation
from Solutions with Non-aqueous Solvents . . . . . . . . . . 346
10.5.4 Electrochemistry-Based Transfer Methods
of Graphene and Graphene Oxide Nanosheets . . . . . . . 347
10.5.5 Electrochemical Exfoliation of Various Inorganic
Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 348