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catalysts Article Pulse Electrolysis Technique for Preparation of Bimetal Tin-Containing Electrocatalytic Materials Alexandra Kuriganova 1,*, Marina Kubanova 1, Igor Leontyev 2 , Tatiana Molodtsova 1 and Nina Smirnova 1 1 Platov South Russian State Polytechnic University (NPI), 132 Prosvecheniya Str., 346428 Novocherkassk, Russia Southern Federal University, Str. Zorge 9, 344090 Rostov-on-Don, Russia 2 * Correspondence: kuriganova_@mail.ru Citation: Kuriganova, A.; Kubanova, M.; Leontyev, I.; Molodtsova, T.; Smirnova, N. Pulse Electrolysis Technique for Preparation of Bimetal Tin-Containing Electrocatalytic Materials. Catalysts 2022, 12, 1444. https://doi.org/10.3390/ catal12111444 Academic Editors: Vladimir Guterman, Sergey Belenov and Anastasia Alekseenko Received: 4 October 2022 Accepted: 11 November 2022 Published: 15 November 2022 Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2022 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). Abstract: Platinum–tin-containing materials are the most popular catalysts for processes occurring in fuel cells with direct ethanol oxidation. Pulse electrolysis based on the electrochemical dispersion of platinum electrodes under the influence of alternating pulse current in an alkaline electrolyte made it possible to introduce the tin component into the catalyst in the form of a dopant, an alloy with platinum, and in the form of an oxide phase and evaluate the effect of the form in which tin is present in the catalyst on its microstructural and electrocatalytic characteristics. The introduction of tin into the catalyst generally increases the rate of ethanol electrooxidation; however, with the most prominent effect observed when tin is present in form of an oxide. Keywords: pulse electrolysis; direct ethanol fuel cell; platinum; tin; electrocatalysis; CO stripping 1. Introduction It is well-known that bi- or polymetallic nanostructures [1,2], including tin- and platinum-based nanostructures, are of great interest due to their potential application in fuel cell technologies with direct oxidation of liquid organic fuel [1,3,4]. Tin is known as the most active cocatalyst for the electrochemical oxidation of ethanol on platinum due to higher oxophilicity of Sn surfaces compared to Pt and other metals [5]. The incorporation of tin into a platinum catalyst changes the electrode’s geometric and electronic structure, providing conditions required for complete ethanol oxidation to carbon dioxide [6]. When developing catalytic materials based on metal alloys, in particular, platinum- based alloys, considerable attention is paid to controlling the composition, size, and struc- ture of catalytically active nanoparticles [2,7,8]. However, the preparation of bimetallic nanoparticles is often a technologically complex process that requires the use of high- temperature post-processing of materials, which can lead to sintering and coarsening of catalytically active particles. Tin can be included in the composition of Pt-containing materials in the form of adatoms [9], alloy [10], in the form of tin oxide as a support for Pt nanoparticles [11,12], and as a dopant of Pt nanoparticles [13,14]. Most of the methods for preparing bimetallic electrocatalysts based on platinum and tin belong to the group of bottom-up methods, which do not allow obtaining materials with the same crystallographic properties of the platinum component in order to assess the effect of the type of introduction of the tin component in the composition of a platinum-containing material. Pulse electrolysis has already established itself as an effective method for obtaining both materials based on platinum nanoparticles [15] and tin oxides [16,17] for various applications by dispersion of metal electrodes under the influence of alternating pulse current in aqueous electrolytes. At the same time, due to the highly nonequilibrium conditions that arise in the near-electrode region when alternating pulse current is applied to the electrodes, pulse electrolysis made it possible to obtain non-hydrated crystalline products that do not require high-temperature post-processing techniques. In addition, Catalysts 2022, 12, 1444. https://doi.org/10.3390/catal12111444 https://www.mdpi.com/journal/catalystsPDF Image | Pulse Electrolysis Bimetal Tin-Containing Electrocatalytic
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