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A three‐dimensional (3D) lamellar structure of a poly(styrene‐block‐isoprene) block copolymer was observed at submicrometer and micrometer levels by scanning electron microscopy combined with a focused ion beam (FIB–SEM). The 3D lamellar structure with an exceptionally large periodicity, about 0.1 μm, was successfully reconstructed, and the size of the reconstructed image by FIB–SEM was 6.0 × 6.0 × 4.0 μm3, which was greater than the transmission electron microtomography data, 3.8 × 3.9 × 0.24 μm3, by a factor of about 40. This result indicates that 3D reconstruction using FIB–SEM is quite useful for direct 3D observations, especially analyses of polymeric materials at the submicrometer and micrometer levels. © 2007 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 677–683, 2007

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The mechanism of the carbon nanotube (CNT) formation and its graphitization has not been well understood and is still under controversy. The authors have been studying a new process to form CNTs, where polyynecontaining carbons are heated and irradiated by an electron beam in a transmission electron microscope (TEM). The technique is compatible to an in-situ observation and was applied to a high-resolution TEM (HRTEM) to elucidate the graphitization mechanism. The observation shows that micro-graphenes exist from the beginning of the formation process and develop to form highly ordered graphene layers through fusion and rearrangement of the premature layers, accompanied by evaporation of micro-graphenes. The CNT formation mechanism focusing on its graphitization is presented and discussed.

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