Controlled fabrication of highly ordered platinum nanostructures using pulsed electrodeposition

Pulsed potential (PP) electrodeposition was utilized for the first time to fabricate three-dimensional (3D) platinum (Pt) nanostructures within phytantriol-based double diamond cubic templates, both with or without 20 % w/w Brij-56 as a pore swelling agent. Unlike conventional direct potential (DP) deposition, the PP approach yielded Pt nanostructures with markedly enhanced uniformity and superior lattice ordering. Small Angle X-ray Scattering (SAXS) revealed that PP-grown structures exhibited sharp, well-defined Bragg peaks corresponding to lattice parameters of 134.2 ± 2.1 Å without Brij-56 and 236.7 ± 2.5 Å with 20 % w/w Brij-56, whereas DP-grown structures showed broader, less distinct peaks with smaller lattice parameter (130.7 ± 1.9 Å and 197.1 ± 2.8 Å, respectively). Notably, In-situ SAXS measurements provided real-time insights into the evolution of 3D Pt nanostructures, enabling direct monitoring of orientational and lateral ordering within the templated phases. High resolution SEM further confirmed the superior quality of PP-grown structures, revealing highly ordered 3D nanowire network with uniform pore sizes of 89.5 ± 1.3 (without Brij-56) and 102.0 ± 0.7 Å (with 20 % w/w Brij-56). Overall, these findings highlight the effectiveness of PP electrodeposition in mitigating structural inhomogeneities, establishing it as a powerful strategy for fabricating well-ordered 3D Pt nanostructures.