We here investigate how the synthesis method affects the crystallite size and atomic structure of cobalt iron oxide nanoparticles. By using a simple solvothermal method, we first synthesized cobalt ferrite nanoparticles of 2 and 7 nm, characterized by Transmission Electron Microscopy (TEM), Small Angle X-ray scattering (SAXS), X-ray and neutron total scattering. The smallest particle size corresponds to only a few spinel unit cells.
View Article and Find Full Text PDFSurfactant-free colloidal syntheses in aqueous media are attractive to develop nanomaterials relevant for various applications, e. g. catalysis or medicine.
View Article and Find Full Text PDFUnderstanding the structure of nanoparticles under (electro)catalytic operating conditions is crucial for uncovering structure-property relationships. By combining X-ray total scattering and pair distribution function analysis with small-angle X-ray scattering (SAXS), we obtained comprehensive structural information on ultrasmall (<3 nm) iridium nanoparticles and tracked their changes during oxygen evolution reaction (OER) in acid. When subjected to electrochemical conditions at reducing potentials, the metallic Ir nanoparticles are found to be decahedral.
View Article and Find Full Text PDFAdvanced in situ analyses are indispensable for comprehending the catalyst aging mechanisms of Pt-based PEM fuel cell cathode materials, particularly during accelerated stress tests (ASTs). In this study, a combination of in situ small-angle and wide-angle X-ray scattering (SAXS & WAXS) techniques were employed to establish correlations between structural parameters (crystal phase, quantity, and size) of a highly active skeleton-PtCo (sk-PtCo) catalyst and their degradation cycles within the potential range of the start-up/shut-down (SUSD) conditions. Despite the complex case of the sk-PtCo catalyst comprising two distinct fcc alloy phases, our complementary techniques enabled in situ monitoring of structural changes in each crystal phase in detail.
View Article and Find Full Text PDFPrecious metal nanoparticles are key for a range of applications ranging from catalysis and sensing to medicine. While gold (Au), silver (Ag), platinum (Pt), palladium (Pd) or ruthenium (Ru) nanoparticles have been widely studied, other precious metals are less investigated. Osmium (Os) is one of the least studied of the precious metals.
View Article and Find Full Text PDFState-of-the-art industrial electrocatalysts for the oxygen evolution reaction (OER) under acidic conditions are Ir-based. Considering the scarce supply of Ir, it is imperative to use the precious metal as efficiently as possible. In this work, we immobilized ultrasmall Ir and IrRu nanoparticles on two different supports to maximize their dispersion.
View Article and Find Full Text PDFGold nanoparticles (Au NPs) and gold-based nanomaterials combine unique properties relevant for medicine, imaging, optics, sensing, catalysis, and energy conversion. While the Turkevich-Frens and Brust-Schiffrin methods remain the state-of-the-art colloidal syntheses of Au NPs, there is a need for more sustainable and tractable synthetic strategies leading to new model systems. In particular, stabilizers are almost systematically used in colloidal syntheses, but they can be detrimental for fundamental and applied studies.
View Article and Find Full Text PDFIridium nanoparticles are important catalysts for several chemical and energy conversion reactions. Studies of iridium nanoparticles have also been a key for the development of kinetic models of nanomaterial formation. However, compared to other metals such as gold or platinum, knowledge on the nature of prenucleation species and structural insights into the resultant nanoparticles are missing, especially for nanoparticles obtained from IrCl precursors investigated here.
View Article and Find Full Text PDFHerein, we report a straightforward approach for the preparation of Pt-Au alloy nanoparticles from Pt + Au/C nanocomposites using monometallic colloidal nanoparticles as starting blocks. Four different compositions with fixed Pt content and varying Pt to Au mass ratios from 1:1 up to 1:7 were prepared as formic acid oxidation reaction (FAOR) catalysts. The study was carried out in a gas diffusion electrode (GDE) setup.
View Article and Find Full Text PDFIntermetallic nanoparticles (NPs) have shown enhanced catalytic properties as compared to their disordered alloy counterparts. To advance their use in green energy, it is crucial to understand what controls the formation of intermetallic NPs over alloy structures. By carefully selecting the additives used in NP synthesis, it is here shown that monodisperse, intermetallic PdCu NPs can be synthesized in a controllable manner.
View Article and Find Full Text PDFAdv Colloid Interface Sci
May 2022
Precious metals are key in various fields of research and precious metal nanomaterials are directly relevant for optics, catalysis, pollution management, sensing, medicine, and many other applications. Iridium based nanomaterials are less studied than metals like gold, silver or platinum. A specific feature of iridium nanomaterials is the relatively small size nanoparticles and clusters easily obtained, e.
View Article and Find Full Text PDFBeilstein J Nanotechnol
February 2022
A surfactant-free synthesis of precious metal nanoparticles (NPs) performed in alkaline low-boiling-point solvents has been recently reported. Monoalcohols are here investigated as solvents and reducing agents to obtain colloidal Os nanoparticles by using low-temperature (<100 °C) surfactant-free syntheses. The effect of the precursor (OsCl or HOsCl), precursor concentration (up to 100 mM), solvent (methanol or ethanol), presence or absence of a base (NaOH), and addition of water (0 to 100 vol %) on the resulting nanomaterials is discussed.
View Article and Find Full Text PDFThe development of nanomaterials often relies on wet-chemical synthesis performed in reflux setups using round-bottom flasks. Here, an alternative approach to synthesize nanomaterials is presented that uses glass tubes designed for NMR analysis as reactors. This approach uses less solvent and energy, generates less waste, provides safer conditions, is less prone to contamination, and is compatible with high-throughput screening.
View Article and Find Full Text PDFHydrogen production from renewable resources and its reconversion into electricity are two important pillars toward a more sustainable energy use. The efficiency and viability of these technologies heavily rely on active and stable electrocatalysts. Basic research to develop superior electrocatalysts is commonly performed in conventional electrochemical setups such as a rotating disk electrode (RDE) configuration or H-type electrochemical cells.
View Article and Find Full Text PDFThe polyol synthesis is a well-established method to form so-called "surfactant-free" nanoparticles (NPs). In the present study, the NP size resulting from the thermal reduction of the precursors HPtCl, HPt(OH), or Pt(acac) in presence of the bases NaOH or Na(acac) at different concentrations is studied. It is shown that the size control depends more strongly on the nature of the precursor (metal salt) than on the anion present in the base.
View Article and Find Full Text PDFUnderstanding the formation of nanomaterials down to the atomic level is key to rational design of advanced materials. Despite their widespread use and intensive study over the years, the detailed formation mechanism of platinum (Pt) nanoparticles remains challenging to explore and rationalize. Here, various characterization techniques, and in particular X-ray total scattering with pair distribution function (PDF) analysis, are used to follow the structural and chemical changes taking place during a surfactant-free synthesis of Pt nanoparticles in alkaline methanol.
View Article and Find Full Text PDFBeilstein J Nanotechnol
December 2020
Controlling the 3D assembly of individual nanomaterials can be a challenging task. However, it opens up opportunities for the production of increasingly complex nanostructures. Unusual rolled multiwall carbon nanotube structures are synthesized here by simply inducing a change of precursor composition during the growth of multiwall carbon nanotube forests.
View Article and Find Full Text PDFFlow reactors are expected to play an increasingly important role in the production of chemicals. A simple carbon-based scaffold to easily develop flow systems is here detailed. Using a chemical vapour deposition technique, the controlled growth of vertically aligned (VA) multi-wall carbon nanotubes (MWCNTs) into quartz columns with 2 mm inner diameter is achieved.
View Article and Find Full Text PDFAdv Colloid Interface Sci
December 2020
Platinum (Pt) is one of the most studied materials in catalysis today and considered for a wide range of applications: chemical synthesis, energy conversion, air treatment, water purification, sensing, medicine etc. As a limited and non-renewable resource, optimized used of Pt is key. Nanomaterial design offers multiple opportunities to make the most of Pt resources down to the atomic scale.
View Article and Find Full Text PDFSeveral concepts for platinum-based catalysts for the oxygen reduction reaction (ORR) are presented that exceed the US Department of Energy targets for Pt-related ORR mass activity. Most concepts achieve their high ORR activity by increasing the Pt specific activity at the expense of a lower electrochemically active surface area (ECSA). In the potential region controlled by kinetics, such a lower ECSA is counterbalanced by the high specific activity.
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