Structural Characterization of Surfactant-Coated Bimetallic Cobalt/Nickel Nanoclusters by XPS, EXAFS, WAXS, and SAXS
Cobalt−nickel bimetallic nanoparticles were synthesized by changing the sequence of the chemical reduction of Co(II) and Ni(II) ions confined in the core of bis(2-ethylhexyl)phosphate 2, and Ni(DEHP)2. The reduction was carried out by mixing, sequentially or contemporaneously, fixed amounts of n-hep...
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Veröffentlicht in: | Journal of physical chemistry. C 2011-04, Vol.115 (14), p.6360-6366 |
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Sprache: | eng |
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Zusammenfassung: | Cobalt−nickel bimetallic nanoparticles were synthesized by changing the sequence of the chemical reduction of Co(II) and Ni(II) ions confined in the core of bis(2-ethylhexyl)phosphate 2, and Ni(DEHP)2. The reduction was carried out by mixing, sequentially or contemporaneously, fixed amounts of n-heptane solution of Co(DEHP)2 and Ni(DEHP)2 micelles with a solution of sodium borohydride in ethanol at a fixed (reductant)/(total metal) molar ratio. This procedure involves the rapid formation of surfactant-coated nanoparticles, indicated as Co/Ni (Co after Ni), Ni/Co (Ni after Co), and Co + Ni (simultaneous), followed by their slow separation as nanostructures embedded in a sodium bis(2-ethylhexyl)phosphate matrix. The resulting composites, together with those obtained by reducing the n-heptane solutions of pure Co(DEHP)2 or Ni(DEHP)2, were characterized by XPS, EXAFS, WAXS, and SAXS. The data analysis confirms the presence of nanometer-sized surfactant-coated cobalt, nickel, and cobalt/nickel particles. As expected, the composition and internal structure of cobalt/nickel bimetallic nanoparticles are influenced by the preparation sequence as well as by the “chemical affinity” between the surfactant and the metal. However, some atomic-scale physicochemical processes play a subtle role in determining the structural features of bimetallic nanoparticles. Further effects due to the competition between nanoparticle growing process and surfactant adsorption at the nanoparticle surface were observed. |
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ISSN: | 1932-7447 1932-7455 |
DOI: | 10.1021/jp200288y |