Abstract
Oleylamine (OA) based “hot injection” colloidal synthesis offers a versatile approach to the synthesis of highly monodisperse metallic and multi-metallic alloyed nanostructures in the absence of potentially toxic and unstable phosphine compounds. For application in heterogeneous catalysis and electrocatalysis, the adsorbed OA species at the metal surfaces should be effectively removed without compromising the structure and composition of the nanostructures. Herein, we investigate the removal of OA from colloidal Pt nanoparticles through 1) “chemical methods” such as washing in acetic acid or ethanol, and ligand exchange with pyridine; and 2) thermal pre-treatment between 185 and 400 °C in air, H2 or Ar atmospheres. The electrochemical reactivity of Pt nanoparticles is acutely affected by the presence of surface organic impurities, making this material ideal for monitoring the effectiveness of OA removal. The results showed that thermal treatment in Ar at temperatures above 400 °C provides highly active particles, with reactivity comparable to the benchmark commercial catalyst, Pt/ETEK. The mechanism involved in thermal desorption of OA was also investigated by thermogravimetric analysis coupled to mass spectrometry (TGA-MS). Oxidation of HCOOH and adsorbed CO in acidic solution were used as test reactions to assess the Pt electrocatalytic activity.
Highlights
Electrocatalysts typically consist of a catalytically active component, such as metallic nanoparticles, incorporated into a support material, often carbon[1,2] or metal oxides (e.g., WO3, TiO2).[3]
Analysis of the Transmission electron microscopy (TEM) micrographs resulted in average size of 3.5 Æ 0.2 nm, in excellent agreement with the value obtained by use of the Scherrer equation in conjunction with the powder X-ray diffraction (XRD) pattern (Figure 1)
The present analysis focuses on Pt nanostructures, our conclusions are relevant to the large range of materials that can be synthesised by “hot injection” in the presence of OA
Summary
Electrocatalysts typically consist of a catalytically active component, such as metallic nanoparticles, incorporated into a support material, often carbon (mesoporous, nanotubes, graphene, diamond)[1,2] or metal oxides (e.g., WO3, TiO2).[3]. The efficacies of several chemical and thermal pre-treatment methods were assessed in terms of changes to the nanoparticle surface and the impact of their electrocatalytic properties with regards to HCOOH and surface-adsorbed CO (COads) oxidation in acidic solution.
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