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Structure and properties of C60-Pd films formed by electroreduction of C60 and palladium(II) acetate trimer: evidence for the presence of palladium nanoparticles
de Bettencourt-Dias, Ana
Sobczak, Janusz W.
Balch, Alan L.
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The compn., surface morphol., structure, and electrochem. properties of thin solid films of the polymer, C60-Pd, were studied by Raman spectroscopy, XPS, powder X-ray diffraction (XRD), and energy dispersive X-ray fluorescence (EDXRF) as well as being examd. by SEM (SEM), high resoln. transmission electron microscopy (HRTEM) with selective area diffraction (SAD) and by cyclic voltammetry (CV), resp. The C60-Pd films were deposited onto Au or Pt electrodes by electroreductive co-polymn. of C60 and the palladium(ii) acetate trimer, [Pd(ac)2]3, in a mixed acetonitrile-toluene (4:1, vol./vol.) soln. of 0.1 M tetra(n-butyl)ammonium perchlorate under multicyclic voltammetry or potentiostatic conditions. The structure and compn. of the C60-Pd films were dependent on the relative concn. of the polymer precursors, i.e., C60 and [Pd(ac)2]3, in the soln. for electropolymn. That is, in films grown in solns. with a high [Pd(ac)2]3:C60 ratio, (-C60-Pd-)n polymeric chains were sepd. by the Pd nanoclusters. These films were relatively smooth and uniform. In contrast, films electropolymd. in solns. with a low [Pd(ac)2]3:C60 ratio were rough, porous and much less uniform. The presence of the Pd nanoclusters in the C60-Pd film influenced the electrode processes of probing redox species dissolved in soln. That is, electro-oxidn. of an N,N,N',N'-tetramethyl-1,4-phenylenediamine (TMPDA) electrochem. redox probe was partially inhibited at the electrode coated by the C60-Pd film with a relatively low Pd nanocluster content. In contrast, electro-oxidn. of TMPDA was effectively mediated by the C60-Pd film contg. appreciable amts. of dispersed Pd nanoclusters.