Ionic Conductivity Measurements—A Powerful Tool for Monitoring Polyol Reduction Reactions

Autor: Klaus F. Wagenbauer, Melanie Miller, Veronika M. Burger, Hany A. El-Sayed, Hubert A. Gasteiger, Manuel Wagenhofer
Rok vydání: 2017
Předmět:
Zdroj: Langmuir. 33:13615-13624
ISSN: 1520-5827
0743-7463
DOI: 10.1021/acs.langmuir.7b03444
Popis: The reduction of metal precursors during the polyol synthesis of metal nanoparticles was monitored by ex situ ionic conductivity measurements. Using commonly used platinum precursors (K2PtCl6, H2PtCl6, and K2PtCl4) as well as iridium and ruthenium precursors (IrCl3 and RuCl3), we demonstrate that their reduction in ethylene glycol at elevated temperatures is accompanied by a predictable change in ionic conductivity, enabling a precise quantification of the onset temperature for their reduction. This method also allows detecting the onset temperature for the further reaction of ethylene glycol with HCl produced by the reduction of chloride-containing metal precursors (at ≈120 °C). On the basis of these findings, we show that the conversion of the metal precursor to reduced metal atoms/clusters can be precisely quantified, if the reaction occurs below 120 °C, which also enables a distinction between the stages of metal particle nucleation and growth. The latter is demonstrated by the reduction of H2PtCl6 in...
Databáze: OpenAIRE