After oxidation, the solution was centrifuged, decanted, and filtered through a 0.2 lm filter to remove silver particles, and freeze-dried for storage. Polyvinylferrocene homopolymer and ferrocene were oxidized in the same manner.Crosslinking: The freeze-dried FTI copolymer was molded mechanically into disks with diameter = 7 mm and thickness = 1 mm. Electron-beam crosslinking of the polymer was performed using an electron-beam source at Tyco Electronics in Menlo Park, CA. The samples were irradiated by a 3 MeV beam source using a series of approximately 0.9 s exposures for a total exposure time of 19.8 s.Transmission Electron Microscopy: Thin sections (ca. 50 nm) of crosslinked FTI were cryomicrotomed at ±100 C and examined by transmission electron microscopy at the National Center for Electron Microscopy at Lawrence Berkeley National Laboratory (LBNL). Staining was not required, since the electron contrast between the iron-containing block and the organic block was sufficient to differentiate the microphases of the polymer.Activity Measurements: Equimolar mixtures of reactants (0.29 mL MVK and 0.50 mL E2OC) were added to 2 mL of solvent (6:1 by volume dichloromethane:methanol mixture). Predetermined amounts of catalysts were added at time zero (t = 0) to the reaction mixture. The swollen crosslinked FTI catalyst was added as cubes approximately 1 mm in length. The Michael addition reaction was carried out in a glass reaction vessel at room temperature in an argon atmosphere. Samples were pipetted out of the glass reactor at regular intervals and analyzed by 1 H NMR. The progress of the reaction was followed by the time dependence of the vinyl proton NMR signal at 6.3 ppm, which is proportional to the concentration of the MVK. The samples obtained from the homogeneous catalysts were filtered through alumina columns to remove the dissolved iron species that interfere with the NMR experiments. In the case of the crosslinked FTI catalyst, no iron removal was needed prior to the NMR analysis. Since 10 % of the ferrocene in FTI remained after oxidation of the ferrocene to ferrocenium, and a small amount of silver may have been trapped in the block copolymer after filtration, experiments were carried out to determine whether ferrocene or silver are catalytically active. Neither of these components was found to be active for Michael addition under the conditions used for this work.