Colloidal platinum nanoparticles are obtained via a surfactant-free polyol process in alkaline ethylene glycol. In this popular synthesis, ethylene glycol functions as solvent and reducing agent. The preparation procedure is known for its reproducibility to obtain 1-2 nm nanoparticles, but at the same time the controlled preparation of larger nanoparticles is challenging. A reliable size control without the use of surfactants is a fundamental yet missing achievement for systematic investigations. In this work it is demonstrated how the molar ratio between NaOH and the platinum precursor determines the final particle size and how this knowledge can be used to prepare and study in a systematic way supported catalysts with defined size and Pt to carbon ratio. Using small-angle X-ray scattering, transmission electron microscopy, infrared spectroscopy, X-ray absorption spectroscopy, pair distribution function and electrochemical analysis it is shown that changing the NaOH/Pt molar ratio from 25 to 3, the Pt nanoparticle size is tuned from 1 to 5 nm. This size range is of interest for various catalytic applications, such as the oxygen reduction reaction (ORR). Supporting the nanoparticles onto a high surface area carbon, we demonstrate how the particle size effect can be studied keeping the Pt to carbon ratio constant, an important aspect that in previous studies could not be accomplished.
Compared to conventional preparation methods for supported heterogeneous catalysts, the use of colloidal nanoparticles (NPs) allows for a precise control over size, size distribution, and distribution/location of the NPs on the support. However, common colloidal syntheses have restrictions that limit their applicability for industrial catalyst preparation. We present a simple, surfactant‐free, and scalable preparation method for colloidal NPs to overcome these restrictions. We demonstrate how precious‐metal NPs are prepared in alkaline methanol, how the particle size can be tuned, and how supported catalysts are obtained. The potential of these colloids in the preparation of improved catalysts is demonstrated by two examples from heterogeneous catalysis and electrocatalysis.
We present studies of the structural and magnetic properties of core-shell ironiron oxide nanoparticles. α-Fe nanoparticles were fabricated by sputtering and subsequently covered with a protective nanocrystalline oxide shell consisting of either maghaemite (γ -Fe 2 O 3 ) or partially oxidized magnetite (Fe 3 O 4 ). We observed that the nanoparticles were stable against further oxidation, and Mössbauer spectroscopy at high applied magnetic fields and low temperatures revealed a stable form of partly oxidized magnetite. The nanocrystalline structure of the oxide shell results in strong canting of the spin structure in the oxide shell, which thereby modifies the magnetic properties of the coreshell nanoparticles.
We show that antiferromagnetic nanoparticles of ␣-Fe 2 O 3 ͑hematite͒ under wet conditions can attach into chains along a common ͓001͔ axis. Electron microscopy shows that such chains typically consist of two to five particles. X-ray and neutron diffraction studies show that both structural and magnetic correlations exist across the interfaces along the ͓001͔ direction. This gives direct evidence for exchange coupling between particles. Exchange coupling between nanoparticles can suppress superparamagnetic relaxation and it may play a role for attachment along preferred directions. The relations between exchange coupling, magnetic properties, and oriented attachment are discussed.
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