Synthesis and characterization of metal–rich phosphonium polyelectrolytes and their use as precursors to nanomaterials

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Abstract

A unique family of polyelectrolytes with four different stoichiometric Fe/Ru ratios were prepared and characterized. Pyrolysis in a reducing atmosphere led to crystalline, mixed phase nanomaterials containing iron, ruthenium, and phosphorus with compositions influenced by the structure of the parent polyelectrolytes.

Abstract

Upon efficient quaternization and salt metathesis of stable triethyl ferrocene/ruthenocene phosphines, styrene-based phosphonium triflate monomers with four different stoichiometric ratios of Fe/Ru were synthesized. Free-radical polymerization of the monomers afforded four polyelectrolytes ( M _n: 38 650–69 100 g mol ⁻¹, Đ: 3.16–4.10) that retained many of the spectroscopic and electrochemical properties of the ferrocene/ruthenocene units. TGA studies demonstrated the thermal stability (onset of decomposition: ∼310 °C) and high char yields (33–54% at 1000 °C) of the polyelectrolytes. Pyrolysis in N ₂/H ₂ (95/5) (film thickness of ∼6 μm, 1000 °C, 3 h) yielded crystalline, mixed-phase nanomaterials containing iron, ruthenium, and phosphorus with compositions influenced by the structure of the parent polyelectrolytes.

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Monodisperse FePt nanoparticles and ferromagnetic FePt nanocrystal superlattices

Sun, Murray, Weller … (2000)

Synthesis of monodisperse iron-platinum (FePt) nanoparticles by reduction of platinum acetylacetonate and decomposition of iron pentacarbonyl in the presence of oleic acid and oleyl amine stabilizers is reported. The FePt particle composition is readily controlled, and the size is tunable from 3- to 10-nanometer diameter with a standard deviation of less than 5%. These nanoparticles self-assemble into three-dimensional superlattices. Thermal annealing converts the internal particle structure from a chemically disordered face-centered cubic phase to the chemically ordered face-centered tetragonal phase and transforms the nanoparticle superlattices into ferromagnetic nanocrystal assemblies. These assemblies are chemically and mechanically robust and can support high-density magnetization reversal transitions.

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Nanoparticles as recyclable catalysts: the frontier between homogeneous and heterogeneous catalysis.

Didier Astruc, Feng Lu, Jaime Ruiz Aranzaes (2005)

Interest in catalysis by metal nanoparticles (NPs) is increasing dramatically, as reflected by the large number of publications in the last five years. This field, "semi-heterogeneous catalysis", is at the frontier between homogeneous and heterogeneous catalysis, and progress has been made in the efficiency and selectivity of reactions and recovery and recyclability of the catalytic materials. Usually NP catalysts are prepared from a metal salt, a reducing agent, and a stabilizer and are supported on an oxide, charcoal, or a zeolite. Besides the polymers and oxides that used to be employed as standard, innovative stabilizers, media, and supports have appeared, such as dendrimers, specific ligands, ionic liquids, surfactants, membranes, carbon nanotubes, and a variety of oxides. Ligand-free procedures have provided remarkable results with extremely low metal loading. The Review presents the recent developments and the use of NP catalysis in organic synthesis, for example, in hydrogenation and C--C coupling reactions, and the heterogeneous oxidation of CO on gold NPs.