"Nano Lab" Advanced Characterization Platform for Studying Electrocatalytic Iridium Nanoparticles Dispersed on TiO x N y Supports Prepared on Ti Transmission Electron Microscopy Grids

被引：6

作者：

Bele, Marjan ^{[1
]}

Podborsek, Gorazd Koderman ^{[1
,2
]}

Loncar, Anja ^{[1
,3
]}

Jovanovic, Primoz ^{[1
]}

Hrnjic, Armin ^{[1
,3
]}

Marinko, Ziva ^{[2
,4
]}

Kovac, Janez ^{[5
]}

Surca, Angelja Kjara ^{[1
]}

Kamscek, Ana Rebeka ^{[1
,6
]}

Drazic, Goran ^{[1
,2
]}

Hodnik, Nejc ^{[1
,2
,3
]}

Suhadolnik, Luka ^{[4
,7
]}

机构：

[1] Natl Inst Chem, Dept Mat Chem, Hajdrihova 19, SI-1000 Ljubljana, Slovenia

[2] Jozef Stefan Int Postgrad Sch, Jamova 39, SI-1000 Ljubljana, Slovenia

[3] Univ Nova Gorica, Vipavska 13, SI-5000 Nova Gorica, Slovenia

[4] Jozef Stefan Inst, Dept Nanostruct Mat, Jamova 39, SI-1000 Ljubljana, Slovenia

[5] Joz?ef Stefan Inst, Dept Surface Engn, Jamova 39, SI-1000 Ljubljana, Slovenia

[6] Univ Ljubljana, Fac Chem & Chem Technol, Vecna pot 113, SI-1000 Ljubljana, Slovenia

[7] Univ Trieste, Dept Chem & Pharmaceut Sci, via L Giorgieri 1, I-34127 Trieste, Italy

来源：

ACS APPLIED NANO MATERIALS | 2023年 / 6卷 / 12期

基金：

欧盟地平线“2020”; 欧洲研究理事会;

关键词：

Nano Lab concept; anodic oxidation; IL-TEM; electrocatalysis; oxygen evolutionreaction; iridium nanoparticles; OXYGEN-EVOLUTION REACTION; DEGRADATION; STABILITY; ACID; HYDROGEN; PERFORMANCE; ADSORPTION; REDUCTION; CATALYSTS; CO;

D O I：

10.1021/acsanm.3c01368

中图分类号：

TB3 [工程材料学];

学科分类号：

0805 ; 080502 ;

摘要：

Aiming at speeding up the discovery and understandingof promisingelectrocatalysts, a novel experimental platform, i.e., the Nano Lab, is introduced. It is based on state-of-the-artphysicochemical characterization and atomic-scale tracking of individualsynthesis steps as well as subsequent electrochemical treatments targetingnanostructured composites. This is provided by having the entire experimentalsetup on a transmission electron microscopy (TEM) grid. Herein, theoxygen evolution reaction nanocomposite electrocatalyst, i.e., iridiumnanoparticles dispersed on a high-surface-area TiO x N y support prepared on the Ti TEMgrid, is investigated. By combining electrochemical concepts suchas anodic oxidation of TEM grids, floating electrode-based electrochemicalcharacterization, and identical location TEM analysis, relevant informationfrom the entire composite's cycle, i.e., fromthe initial synthesis step to electrochemical operation, can be studied.We reveal that Ir nanoparticles as well as the TiO x N y support undergo dynamic changesduring all steps. The most interesting findings made possible by the Nano Lab concept are the formation of Ir single atoms andonly a small decrease in the N/O ratio of the TiO x N y -Ir catalyst during theelectrochemical treatment. In this way, we show that the precise influenceof the nanoscale structure, composition, morphology, and electrocatalyst'slocally resolved surface sites can be deciphered on the atomic level.Furthermore, the Nano Lab's experimental setupis compatible with ex situ characterization and otheranalytical methods, such as Raman spectroscopy, X-ray photoelectronspectroscopy, and identical location scanning electron microscopy,hence providing a comprehensive understanding of structural changesand their effects. Overall, an experimental toolbox for the systematicdevelopment of supported electrocatalysts is now at hand.

引用

页码：10421 / 10430

页数：10