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      Continuous mesoporous pd films by electrochemical deposition in nonionic micellar solution

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      Author(s)
      Iqbal, M.
      Li C.
      Wood, K.
      Jiang B.
      Takei, T.
      Dag, Ö.
      Baba, D.
      Nugraha, A. S.
      Asahi, T.
      Whitten, A. E.
      Hossain, M. S. A.
      Malgras, V.
      Yamauchi, Y.
      Date
      2017
      Source Title
      Chemistry of Materials
      Print ISSN
      0897-4756
      Publisher
      American Chemical Society
      Volume
      29
      Issue
      15
      Pages
      6405 - 6413
      Language
      English
      Type
      Article
      Item Usage Stats
      217
      views
      415
      downloads
      Abstract
      Mesoporous metals that combine catalytic activity and high surface area can provide more opportunities for electrochemical applications. Various synthetic methods, including hard and soft templating, have been developed to prepare mesoporous/nanoporous metals. Micelle assembly, typically involved in soft-templates, is flexible and convenient for such purposes. It is, however, difficult to control, and the ordering is significantly destroyed during the metal deposition process, which is detrimental when it comes to designing precisely mesostructured materials. In the present work, mesoporous Pd films were uniformly electrodeposited using a nonionic surfactant, triblock copolymer poly(ethylene oxide)-b-poly(propylene oxide)-b-poly(ethylene oxide), as a pore-directing agent. The interaction between micelles and metal precursors greatly influences the metal growth and determines the final structure. The water-coordinated species interact with the ethylene oxide moiety of the micelles to effectively drive the Pd(II) species toward the working electrode surface. From small-angle neutron scattering data, it is found that spherical P123 micelles, with an average diameter of ∼14 nm, are formed in the electrolyte, and the addition of Pd ions does not significantly modify their structure, which is the essence of the micelle assembly approach. The uniformly sized mesopores are formed over the entire mesoporous Pd film and have an average pore diameter of 10.9 nm. Cross-sectional observation of the film also shows mesopores spanning continuously from the bottom to the top of the film. The crystallinity, crystal phase, and electronic coordination state of the Pd film are also confirmed. Through this study, it is found that the optimized surfactant concentration and applied deposition potential are the key factors to govern the formation of homogeneous and well-distributed pores over the entire film. Interestingly, the as-prepared mesoporous Pd films exhibit superior electrocatalytic activity toward the ethanol oxidation reaction by fully utilizing the accessible active surface area. Our approach combines electrochemistry with colloidal and coordination chemistry and is widely applicable to other promising metals and alloy electrocatalysts.
      Keywords
      Catalyst activity
      Coordination reactions
      Deposition
      Digital storage
      Electrocatalysts
      Electrochemistry
      Electrodeposition
      Electrodes
      Electrolytes
      Ethylene
      Mesoporous materials
      Metals
      Micelles
      Neutron scattering
      Nonionic surfactants
      Oxide films
      Palladium compounds
      Polyethylene oxides
      Reduction
      Surface active agents
      Synthetic metals
      Co-ordination chemistries
      Cross-sectional observations
      Electrocatalytic activity
      Electrochemical applications
      Electrochemical deposition
      Ethanol oxidation reaction
      Mesostructured materials
      Surfactant concentrations
      Palladium
      Permalink
      http://hdl.handle.net/11693/37304
      Published Version (Please cite this version)
      http://dx.doi.org/10.1021/acs.chemmater.7b01811
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      • Institute of Materials Science and Nanotechnology (UNAM) 2258
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