A dispenser-reactor apparatus applied for in situ XAS monitoring of Pt nanoparticle formation

作者:Boita Jocenir; Castegnaro Marcus Vinicius; Martins Alves Maria do Carmo; Morais Jonder*
来源:JOURNAL OF SYNCHROTRON RADIATION, 2015, 22(3): 736-744.
DOI:10.1107/S1600577515003434

摘要

In situ time-resolved X-ray absorption spectroscopy (XAS) measurements collected at the Pt L3-edge during the synthesis of Pt nanoparticles (NPs) in aqueous solution are reported. A specially designed dispenser-reactor apparatus allowed for monitoring changes in the XAS spectra from the earliest moments of Pt ions in solution until the formation of metallic nanoparticles with a mean diameter of 4.9 +/- 1.1 nm. By monitoring the changes in the local chemical environment of the Pt atoms in real time, it was possible to observe that the NPs formation kinetics involved two stages: a reduction-nucleation burst followed by a slow growth and stabilization of NPs. Subsequently, the synthesized Pt NPs were supported on activated carbon and characterized by synchrotron-radiation-excited X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD) and extended X-ray absorption fine structure (EXAFS). The supported Pt NPs remained in the metallic chemical state and with a reduced size, presenting slight lattice parameter contraction in comparison with the bulk Pt values.

  • 出版日期2015-5