KEY WORDSPalladium N anoparticles / Reduction of Palladium Ions/ Poly(2-vinylpyridine)-blockpolyisoprene / Mixtures of Block Copolymers/ Lamella Microdomain / Self-Assembled Structure/ As one of interesting themes in physical science of block copolymers, some groups of researchers have been exploring methods and principles of 'nanoprocessing' of block copolymer microdomain structures. The nanoprocessing involves processings of the microdomains formed in the block copolymers (i) to create 'nanochannels'1 (holes created in one of the microdomain phase dispersed in the matrix of other microdomain phase) or 'nanotextures' 2 (created by selectively removing the matrix phase, while preserving the dispersed phase) and (ii) to create 'nanohybrids' by incorporating nanometal particles, organic or inorganic particles into desired parts of the microdomain space. 3~5 The nanochannels and nanotextures can be coated with metals. 1 The nanoprocessing may involve a processing to create an oriented single grain ofmicrodomain structures. 6 • 7 In this communication we present highlights of our work to create a nanohybrid composed of alternating lamellar microdomains of polyisoprene (PI) and poly(2-vinylpyridine) (P2VP) containing palladium nanoparticles (denoted hereafter by Pd for the sake of simplicity) of ca. 5 nm in diameter selectively in the P2VP lamellae. We will present a novel method to control a spatial distribution of Pd in the P2VP lamellae across the interface. This method, which has never been reported so far to our knowledge, involves firstly a preparation of Pd coordinated and stabilized by poly(2-vinylpyridine)-blockpolyisoprene (Pd-(P2VP-b-PI)) and secondly induces selfassembling of Pd-(P2VP-b-PI) and poly(2-vinylpyridine)-block-polyisoprene (P2VP-b-PI) forming the matrix phase for Pd via solvent casting with benzene. In our earlier report 8 we presented a method to prepare Pd-(P2VP-b-PI) of 4 to 6 nm in diameter. The self-assembly of Pd-(P2VP-b-PI) and P2VP-b-PI block copolymer with chloroform as a solvent was shown to create a nanohybrid in which Pd are selectively localized in the P2VP lamellae. However no methods have been so far proposed to control the location of Pd within the P2VP lamellae, e.g., a uniform distribution of the particles across the interface, or controlled alignment of the particles along the interface or in the middle of the P2VP lamellae etc. This is a point which we would like to address in this paper.A method similar to that described above was presented earlier by Schrock and his coworkers.4 They first prepared a block copolymer having a block which contains P(octyl) 2 side groups and CdSe nanoclusters stabilized by P(octyl)a or O=P(octyl)a. The block copolymers and the CdSe nanoclusters were then solution-cast into films. The CdSe nanoclusters are selectively coordinated in the microdomains comprised of the block chains with P(octylh side groups. However the controlled spatial arrangement of the particles within the microdomains was not reported at all.Here in this work we used t...