In-situ and operando Grazing Incidence XAS: a novel set-up and its application to model Pd electrodes for alcohols oxidation

IF 2 4区化学 Q3 CHEMISTRY, MULTIDISCIPLINARY

Pure and Applied Chemistry Pub Date : 2024-03-08 DOI:10.1515/pac-2023-1013

Enrico Berretti, Andrea Giaccherini, Vincenzo Dell’Aquila, Francesco Di Benedetto, Giordano Montegrossi, Giovanni Orazio Lepore, Massimo Innocenti, Francesco D’Acapito, Francesco Vizza, Alessandro Lavacchi

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引用次数: 0

Abstract

In this article, we present an in-situ and operando time-resolved X-ray Absorption Spectroscopy (XAS) technique which exploits a combination of Grazing Incidence XAS (GIXAS) and Fixed Energy X-ray Absorption Voltammetry (FEXRAV), the Grazing Incidence FEXRAV (GI-FEXRAV). A case-study is also outlined. Palladium ultra-low loadings were deposited above Au polycrystalline iso-oriented substrates adopting three different deposition methods: surface-controlled electrochemical methods, direct electrodeposition, and physical vapour deposition (PVD). These catalytical surfaces were prepared for the investigation by GI-FEXRAV of the Pd oxidation/dissolution phenomenon that could occur when the metal is used in the anodic compartment of Direct Alcohol Fuel Cells (DAFCs) or in electrochemical reformers. Moreover, we report a robust, low cost and versatile procedure to obtain wide and flat iso-oriented gold substrates that can mimic monocrystalline gold (1 1 1) in the electrochemical response. The use of GI-FEXRAV for the operando characterization of the catalysts, in conjunction with the designed experimental cell and our flexible Au-based electrochemical substrates show an invaluable potential in the operando study of fundamental phenomena in heterogeneous electrocatalysis model systems and, due to its versatility, paves the way to further studies on a wide selection of electrochemical systems.

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原位和操作性掠入射 XAS：一种新型装置及其在醇氧化模型钯电极中的应用

在这篇文章中，我们介绍了一种原位和操作时间分辨 X 射线吸收光谱（XAS）技术，该技术结合了掠入射 XAS（GIXAS）和固定能量 X 射线吸收伏安法（FEXRAV），即掠入射 FEXRAV（GI-FEXRAV）。此外，还概述了一个案例研究。采用三种不同的沉积方法：表面控制电化学方法、直接电沉积和物理气相沉积（PVD），在金多晶等取向基底上沉积了超低负载的钯。制备这些催化表面是为了通过 GI-FEXRAV 对 Pd 氧化/溶解现象进行研究，这种现象可能发生在直接酒精燃料电池（DAFC）阳极室或电化学转化炉中使用金属时。此外，我们还报告了一种坚固耐用、成本低廉且用途广泛的方法，用于获得宽而平整的等取向金基板，该基板可在电化学反应中模拟单晶金 (1,1,1)。使用 GI-FEXRAV 对催化剂进行操作表征，结合设计的实验单元和我们灵活的金基电化学基底，显示了在异相电催化模型系统中对基本现象进行操作研究的宝贵潜力，而且由于其多功能性，为进一步研究多种电化学系统铺平了道路。

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来源期刊

Pure and Applied Chemistry 化学-化学综合

CiteScore

4.00

自引率

0.00%

发文量

审稿时长

3-8 weeks

期刊介绍： Pure and Applied Chemistry is the official monthly Journal of IUPAC, with responsibility for publishing works arising from those international scientific events and projects that are sponsored and undertaken by the Union. The policy is to publish highly topical and credible works at the forefront of all aspects of pure and applied chemistry, and the attendant goal is to promote widespread acceptance of the Journal as an authoritative and indispensable holding in academic and institutional libraries.