A neutron reflectivity study on a terraced lamellar morphology in a block copolymer thin film

Ken Ichi Niihara, Ukyo Matsuwaki, Naoya Torikai, Kotaro Satoh, Masami Kamigaito, Hiroshi Jinnai

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3 Citations (Scopus)


A microphase-separated structure of a poly(deuterated styrene-block-2- vinylpyridine) (dPS-b-P2VP) block copolymer thin film was studied by neutron reflectivity (NR). The spun-coated dPS-b-P2VP block copolymer (on a Si substrate) showed the coexistence of a minority thin lamellar layer (holes) dispersed in a majority thick layer. The "terraced structure" was formed due to the mismatch between the initial film thickness and the intrinsic lamellar periodicity of the dPS-6-P2VP block copolymer. The amount and height of the holes were evaluated using atomic force microscopy (AFM), transmission electron microscopy (TEM) and transmission electron microtomography (TEMT). The three-dimensional (3D) images obtained from the TEMT experiments clearly showed that the microphase-separated structure inside the thin film was homeotropically aligned. The thickness of the thick and the thin lamellar layers corresponded to (5/2)L0 and (3/2)L0, respectively (L0 is the lamella periodicity in the bulk state). The NR profile from the dPS-b-P2VP thin film, Rexp, showed many distinctive scattering peaks. Based on the structural information obtained from the microscopy, a scattering length density profile along the depth direction, i.e., the direction normal to the film surface, b/vTEMT was evaluated, which was then used as an initial profile in the conventional model fitting method. An excellent best-fit to Rexp was obtained using b/vTEMT, even though the thin film had the terraced structure. The surface coverage of the holes was estimated from the resulting b/v, which was in good agreement with the estimated value from TEM.

Original languageEnglish
Pages (from-to)1105-1111
Number of pages7
JournalPolymer Journal
Issue number11
Publication statusPublished - 2007


  • Block copolymer
  • Neutron reflectivity
  • Thin film(s)
  • Transmission electron microtomography


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