In this paper we report the results obtained for inter-matrix synthesis (IMS) and characterization of monometallic and bimetallic polymer-stabilized metal nanoparticles (PSMNPs). The IMS procedure is based on the use of appropriately functionalized polymeric membranes as nanoreactors, which allows both synthesis and characterization of the composition and morphology of PSMNPs inside the membranes. The membranes were prepared by using noncrosslinked sulfonated poly(etherether ketone) (SPEEK) of desired degree of sulfonation, which provided insolubility of the polymer in water and solubility in some organic solvents (e.g. dimethylformamide). The IMS of PSMNPs involved loading of the membrane with metal ions or complexes followed by metal reduction inside the membrane resulting in the formation of either monometallic (Cu or Pt) or bimetallic (Pt/Cu) PSMNPs with core–shell structure. The electrocatalytic activity of the PSMNPs was estimated by measuring the electrochemical response of amperometric sensors prepared by using SPEEK-Pt-PSMNP and SPEEK-Pt/Cu-PSMNP nanocomposite membranes as sensing elements to detect H2O2. At the same values of Pt loading the response of Pt/Cu-PSMNP-based sensors appeared to be far higher than that of sensors modified with Pt-PSMNP membranes. (© 2008 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim)

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