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. 2022 Apr 6;12(7):1233.
doi: 10.3390/nano12071233.

Development of a Bifunctional Ti-Based Gas Diffusion Electrode for ORR and OER by One- and Two-Step Pt-Ir Electrodeposition

Maximilian Cieluch  1 , Pit Yannick Podleschny  1 , Norbert Kazamer  1 , Florian Josef Wirkert  1 , Ulrich Wilhelm Rost  1   2 , Michael Brodmann  1
Affiliations

Development of a Bifunctional Ti-Based Gas Diffusion Electrode for ORR and OER by One- and Two-Step Pt-Ir Electrodeposition

Maximilian Cieluch et al. Nanomaterials (Basel). .

Abstract

The present paper presents one- and two-step approaches for electrochemical Pt and Ir deposition on a porous Ti-substrate to obtain a bifunctional oxygen electrode. Surface pre-treatment of the fiber-based Ti-substrate with oxalic acid provides an alternative to plasma treatment for partially stripping TiO2 from the electrode surface and roughening the topography. Electrochemical catalyst deposition performed directly onto the pretreated Ti-substrates bypasses unnecessary preparation and processing of catalyst support structures. A single Pt constant potential deposition (CPD), directly followed by pulsed electrodeposition (PED), created nanosized noble agglomerates. Subsequently, Ir was deposited via PED onto the Pt sub-structure to obtain a successively deposited PtIr catalyst layer. For the co-deposition of PtIr, a binary PtIr-alloy electrolyte was used applying PED. Micrographically, areal micro- and nano-scaled Pt sub-structure were observed, supplemented by homogenously distributed, nanosized Ir agglomerates for the successive PtIr deposition. In contrast, the PtIr co-deposition led to spherical, nanosized PtIr agglomerates. The electrochemical ORR and OER activity showed increased hydrogen desorption peaks for the Pt-deposited substrate, as well as broadening and flattening of the hydrogen desorption peaks for PtIr deposited substrates. The anodic kinetic parameters for the prepared electrodes were found to be higher than those of a polished Ir-disc.

Keywords: Ti-substrate; bifunctional electrode; co- and successive Pt-Ir electrodeposition; electrolysis; fuel cell; micro- and nanostructure; ready to use electrode; unitized regenerative fuel cell; wet-chemical etching.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Topography of the (a) untreated and (b) the calculated porosity Ti-substrate showing its fiber structure and porosity.
Figure 2
Figure 2
Topography of Ti-substrates after (a) plasma and (b) oxalic acid treatment.
Figure 3
Figure 3
Schematic process of the electrode preparation chain, showing the one-step and two-step PtIr deposition method (co- and successive PtIr deposition).
Figure 4
Figure 4
SEM-micrographs of Pt agglomerates obtained via a combined electrochemical deposition method onto Ti-substrate at (a) 5000×, (b) 20,000× and (c) 50,000× magnification.
Figure 5
Figure 5
Cyclic voltammograms of (a) Ti-based electrodes with electrochemical deposited Pt, (b) polished, high purity Pt-disc.
Figure 6
Figure 6
SEM-micrographs of two-step electrodeposited PtIr electrodes at (a) 5000×, (b) 20,000× and (c) 50,000× magnification.
Figure 7
Figure 7
EDX mapping of a two-step deposited PtIr electrode, where (a) shows the selected area for the analysis, (b) the superposed element analysis, (c) the Ir specific analyze and (d) the Pt specific analyze.
Figure 8
Figure 8
Cyclic voltammogram of (a) Ti-based electrode with two-step deposited PtIr, (b) polished, high purity Ir-disc (also shown in inset).
Figure 9
Figure 9
(a) Linear voltammetry for two-step deposited PtIr electrode and (b) OER Tafel plots for two-step deposited PtIr electrode and polished, high purity Ir-disc.
Figure 10
Figure 10
SEM-micrographs of one-step electrodeposited PtIr electrodes at (a) 5000×, (b) 20,000× and (c) 50,000× magnification.
Figure 11
Figure 11
EDX spot analysis of one-step deposited PtIr electrode showing: (a) EDX spectrum obtained for the modified surface spot by pre-treatment and (b) EDX spectrum for a less modified surface spot.
Figure 12
Figure 12
Cyclic voltammogram of (a) Ti-based one-step deposited PtIr electrode and (b) polished, high purity Pt- and Ir-disc (also shown in inset).
Figure 13
Figure 13
(a) Linear voltammetry for one-step deposited PtIr electrode and (b) OER Tafel plots for two-step deposited PtIr electrode and polished high-purity Ir-disc.
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