Electrosynthesis of Iron-Based Metal–Organic Materials with Bis(salicylic acid) Derivatives

• Published in: Journal of physical chemistry. C 2024-07, Vol.128 (28), p.11904-11914
• Main Authors: Realista, Sara, Reis, Ana R., Borralho, Duarte, Corregidor, Victoria, Alves, Luís C., Magalhães, Sérgio, Nunes, Telmo, Viana, Ana S., Pires, João, Ferraria, Ana M., Botelho do Rego, Ana M., Martinho, Paulo N.
• Format: Article
• Language: English
• Subjects: C: Physical Properties of Materials and Interfaces
• ISSN: 1932-7447; 1932-7455
• DOI: 10.1021/acs.jpcc.4c02651

This study examines the electrosynthesis of novel iron-organic films via cathodic electrodeposition using cyclic voltammetry to establish suitable deposition potentials for two different organic linkers: 2,5-dihydroxyterephthalic acid (DOBDC) and 3,3′-dihydroxybiphenyl-4,4′-dicarboxylic acid (BPP). The synthesis process focuses on the coordination of carboxylate to iron centers, producing amorphous films. Analytical techniques including infrared spectroscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, atomic force microscopy (AFM), and a combination of particle-induced X-ray emission and Rutherford backscattering spectrometry were employed to characterize the films’ chemical, morphological, and structural properties. AFM analysis highlighted the evolution of film morphology with deposition time, revealing a transition from highly ordered to more random structures, influencing film crystallinity. Electrochemical assessments demonstrated the stability and electroactive nature of the films, with their behavior dependent on the specific linker used, reflected in the varied electrochemical responses and film properties observed. The study not only refines the synthesis process for metal–organic films but also delineates the impact of synthesis parameters such as linker type, deposition time, and applied potential on the properties of the resulting materials, paving the way for future investigations into diverse electrosynthesis conditions and deprotonation mechanisms for creating innovative metal–organic materials.