Lab-made 3D-printed accessories for spectroscopy and spectroelectrochemistry: a proof of concept to investigate dynamic interfacial and surface phenomena.

Abstract

3D printing is presentedas an auspicious additive manufacturing technique for diverse interesting applications coupling electrochemistry and spectroscopy techniques, proposing as utilities: a general-purpose module for specular spectroscopy and spectroelectrochemical (SEC) cells for in situ UV-VIS and Raman measures capable of acting in flux or a stationary regime. As a proof of concept, UV-VIS absorption and middle-infrared spectra of an azo dye thin film were collected with the specular module showing characteristic bands according to the literature data. SEC investigations related to the Prussian Blue (PB) film growth on the platinum electrode surface were also investigated. By applying appropriate potentials, the PB film growth was accompanied by a proportional increase in the absorption signal at 700 nm in the UV-VIS region. This signal was related to the intervalence charge transfer from the Fe(II)-C to Fe(III)-N. Moreover, the Raman SEC experiment presented scattering intensity at 2092 and 2156 cm-1, related to the (CN) mode associated with the Fe(II) and Fe(III) cations, which was observed during the thin film growth. In addition, the conversion to the Berlin Green (BG) and Prussian White (PB) forms was monitored while applying the suitable potential and in situ spectroscopic observations of structural changes during the redox processes were also detected as described in the literature. Thus, it is possible to state that the accessories successfully validated in situ spectroelectrochemical dynamic investigations unlocking many other applications in this research field.